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Spherical magnesium halide adduct and preparation method and application thereof
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A technology of magnesium halides and adducts, applied in the direction of magnesium organic compounds, etc.
Active Publication Date: 2012-11-28
CHINA PETROLEUM & CHEM CORP +1
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However, the magnesium halide adduct prepared according to the method of this patent application has a large amount of irregular particles, such as needle-shaped particles and rod-shaped particles, and when the catalyst using the magnesium halide adduct as a carrier is used for olefin polymerization, it will undoubtedly cause The resulting polymer also has a large number of irregular particles
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[0024] According to one embodiment of the present invention, the spherical magnesium halide adduct may or may not contain o-hydroxybenzoate and / or polyol ester. In this case, the spherical magnesium halide adduct can be represented by the general formula MgXY-mROH-nCH 3 OH-sG-tDOE-qH 2 O represents, wherein, MgXY, ROH, m, n and q are all the same as the above definitions, G represents o-hydroxybenzoate, s is 0-0.05, DOE represents polyol ester, and t is 0-0.1. When s and t are all 0 (that is, the spherical magnesium halide adduct does not contain o-hydroxybenzoate and polyol ester), the general formula MgXY-mROH-nCH 3 OH-sG-tDOE-qH 2 O is equivalent to the general formula MgXY-mROH-nCH 3 OH-qH 2 O; when t is 0, but s is not 0 (that is, the spherical magnesium halide adduct contains o-hydroxybenzoate, but does not contain polyol ester), the general formula MgXY-mROH-nCH 3 OH-sG-tDOE-qH 2 O is equivalent to the general formula MgXY-mROH-nCH 3 OH-sG-qH 2 O; when s is 0, b...
Embodiment 1
[0060] This example is used to illustrate the spherical magnesium halide adduct provided by the present invention and its preparation method and application.
[0061] (1) Preparation of spherical magnesium chloride adduct
[0062] In a 300L autoclave, add 90L of white oil, 90L of silicone oil, 9.0kg of magnesium chloride (94.7mol) and 14.5L of ethanol (249.0mol), raise the temperature to 125°C under stirring, and stir at 125°C for 2.5 Hour, then, the mixed liquid obtained enters in the hexane that is cooled to-30 ℃ in advance after being fully sheared and dispersed by the high-gravity rotating bed, filters off liquid, and washes five times with hexane, obtains the solid matter of 18kg after drying ( Alcoholate of magnesium chloride).
[0063] In a 1.6L reactor, add 900ml of hexane, add 90 grams of the above-mentioned solid matter, and then dissolve 45ml of dimethoxypropane solution (dimethoxypropane) in 180ml of hexane The content is 0.37mol) was added therein, then, the tem...
Embodiment 2
[0070] This example is used to illustrate the spherical magnesium halide adduct provided by the present invention and its preparation method and application.
[0071] Preparation of spherical magnesium chloride adduct, preparation of olefin polymerization catalyst, and polymerization of propylene were carried out in the same manner as in Example 1, except that the amount of hydrogen added during the polymerization of propylene was 5.0 L.
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Abstract
The invention provides a spherical magnesiumhalideadduct and a preparation method thereof. The method comprises the following steps of: (1) mixing magnesiumhalide and alcohols except methanol with optional inert liquid media and heating the obtained mixture under stirring until a melt of the magnesiumhalideadduct is formed; (2) adding the melt of the magnesium halide adduct to cooling media after shearing and dispersing the melt to form spherical solid particles; and (3) carrying out contact reaction on the spherical solid particles and dimethoxy propane in the inert dispersion media. The invention also provides application of the magnesium halide adduct as a catalyst carrier. The magnesium halide adduct has the following beneficial effects: the morphology of particles of the magnesium halide adduct is more regular and is basically spherical; the particle size distribution is more concentrated; basically special-shaped particles do not exist; and the catalyst prepared by adopting the spherical magnesium halide adduct as the catalyst carrier has better hydrogen regulation sensitivity in propylene polymerization reaction.
Description
technical field [0001] The present invention relates to a spherical magnesium halide adduct, a preparation method of the spherical magnesium halide adduct, a spherical magnesium halide adduct prepared by the method, and an application of the spherical magnesium halide adduct as a catalyst carrier . Background technique [0002] The preparation of Ziegler-Natta catalysts by supporting titanium compounds and electron donor compounds on active magnesium halides is well known in the prior art. Usually, the active magnesium halide uses an adduct of magnesium halide and alcohol, which is used as a carrier to react with titanium halide and an electron donor compound to obtain a spherical catalyst. When the spherical catalyst is used for olefin polymerization (especially propylene polymerization), it has high polymerization activity and stereospecificity, and the obtained polymer has good particle shape. [0003] The disclosed adducts of magnesium halides and alcohols generally in...
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