Preparation method of catalyst solid component for olefin polymerization
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A technology for olefin polymerization and solid components, which is applied in the field of preparation of catalyst solid components for olefin polymerization, and can solve the problems of complex catalyst preparation process, low isotacticity of products, damage to male reproductive system and human immune system, etc.
Inactive Publication Date: 2016-04-20
CHNA ENERGY INVESTMENT CORP LTD +2
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Problems solved by technology
[0008] Both JP2001-114811A and JP2003-040918A use magnesium alkoxide as raw material, and the cost is relatively high
In addition, the hydrogen adjustment sensitivity of the catalyst prepared by alkoxymagnesium is low
[0009] Although the above-mentioned documents disclose that some non-aromatic ester compounds can be used as internal electron donors in the preparation of catalysts, the preparation process of catalysts is very complicated and the yield is low
[0010] It is concluded that the prior art has the following defects in the preparation of catalyst solid components for olefin polymerization: (1) most of the internal electron donors used are plasticizers, which have potential safety hazards and can interfere with the endocrine of humans and animals , can damage the male reproductive system and the human immune system; (2) When using electron donors other than plasticizers, the final polymerization product has low isotacticity and poor performance; (3) Alkanes are used in the raw materials Magnesium oxide, the cost is higher; (4) the preparation process is complicated, and the yield is lower
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Embodiment 1
[0079] (1) alcoholate preparation:
[0080] 5 g (about 0.05 mol) of anhydrous magnesium chloride, 23 mL (about 0.15 mol) of isooctyl alcohol, 30 mL (about 0.15 mol) of dry decane, 2 mL (about 0.0074 mol) of 1-cyclohexene-4,5-dicarboxylic acid Add di-n-butyl ester, 2.5g (about 0.0074mol) tetrabutyl titanate and 50mL dry toluene into the reaction flask, and react at 120°C for 4 hours under the protection of nitrogen to fully dissolve anhydrous magnesium chloride to obtain a stable and uniform Magnesium halide alcoholate solution.
[0081] (2) Solid catalyst preparation:
[0082] Under a nitrogen atmosphere, cool the homogeneous solution prepared above to -20°C, keep the temperature constant for 30 minutes, and gradually add 100ml (about 0.9mol) of titanium tetrachloride into the reactor within 1 hour. After the addition is complete, after 3.5 hours Raise the temperature to 110°C, add 2.5ml (about 0.0093mol) of di-n-butyl 1-cyclohexene-4,5-dicarboxylate, and react at this tempe...
Embodiment 2-5
[0091] With the add-on of internal electron donor in step (1), step (2), the adding temperature of internal electron donor in step (2) is a variable, and other are all set embodiment 2-5 identically with embodiment 1, its result As shown in Table 1. Among them, " / " represents the unchanged factor.
[0092] The parameter change and experimental result of table 1 embodiment 2-5
[0093]
Embodiment 6
[0095] In Example 1, "1-cyclohexene-4,5-dicarboxylic acid di-n-butyl ester" was replaced by "1,2-dimethylcyclohexene-4,5-dicarboxylic acid diisobutyl ester", All the other are identical with embodiment 1.
[0096] Catalyst composition analysis results:
[0097] Titanium content: 2.65% (wt)
[0098] Magnesium content: 17.4% (wt)
[0099] Ester content: 7.2% (wt);
[0100] Polymerization result: catalytic activity 45,600gPP / gCat, polymer apparent density 0.45g / cm3 , The isotacticity is 97.3%.
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Abstract
The invention provides a preparation method of a catalyst solid component for olefin polymerization. The method comprises: (1) preparing a magnesium halide alcohol adduct solution, namely carrying out reaction on anhydrous magnesium halide, an alcohol compound, titanate and a first part internal electron donor in an alkane or aromatic solvent solution to obtain the magnesium halide alcohol adduct solution; and (2) preparing the catalyst solid component, namely enabling a second part internal electron donor to react with titanium halide and the magnesium halide alcohol adduct solution which is obtained in the step (1) so as to obtain the catalyst solid component, wherein the internal electron donors are the same and are ester compounds with structural formulas shown by the formula 1, and in the formula 1 which is shown in the specification, R1 and R2 are selected from hydrogen atoms, and alkyl groups and naphthenic bases with 1-8 carbon atoms, and R3 and R4 are selected from alkyl groups and naphthenic bases with 1-8 carbon atoms. According to the preparation method provided by the invention, the potential safety hazard of a plasticizing agent to a human body is eliminated, the finally polymerized product is high in isotacticity and high in performance, the cost is reduced, and the process is simple and is high in yield.
Description
technical field [0001] The invention belongs to the field of catalyst preparation, and in particular relates to a method for preparing a catalyst solid component for olefin polymerization. Background technique [0002] Since the advent of Ziegler-Natta catalysts, the preparation methods and related technologies for olefin polymerization catalysts have made great progress. Some olefin polymerization catalysts have been successfully industrialized and applied to various polymerization processes. Most of the Ziegler-Natta catalyst components used in conventional polymerization contact magnesium compounds, titanium compounds, halides and electron donors to form olefin polymerization catalysts. Usually, the electron donor added in the catalyst preparation process is an internal electron donor, such as Chinese patents CN85100997A and CN1172966C. In the case of special requirements for the product, it is also necessary to add an external electron donor compound. [0003] Internal...
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