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Titanium fluoride modified load type chrome alum double-active center catalyst and preparation method thereof

A supported catalyst technology, applied in the field of supported chromium vanadium double-active center catalysts and its preparation, can solve the problems of poor comonomer insertion effect, insignificant improvement of polymerization activity, and inability to improve copolymerization performance, etc.

Inactive Publication Date: 2015-12-30
CHINA PETROLEUM & CHEM CORP
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  • Abstract
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Problems solved by technology

[0009] In the patent (application number 201210118427.2), a new type of supported chromium vanadium metal oxide double-active center ethylene polymerization catalyst is reported, as a representative of the third-generation Phillips catalyst with Cr-V double active center, which is characterized in that it is based on the Phillips chromium series The introduction of supported vanadium active components on the catalyst makes it a chromium-based polyethylene catalyst with two active centers of Cr-V. Unmodified silica gel is used as the catalyst carrier to achieve the purpose of wide relative molecular mass distribution, but the comonomer The insertion effect is not good, and the silica gel patent (Application No. 201210134632.8) has also reported about titanium dioxide-modified supported chromium vanadium metal oxide double-active center polyethylene catalysts. Catalyst preparation is carried out through titanium-modified silica gel, which improves catalyst activity and increases The relative molecular mass distribution width of the polymerized product is improved, but the purpose of improving the copolymerization performance cannot be achieved
Patent (Application No. 201210235852.X) also reported about the fluorine-modified supported chromium-vanadium metal oxide double-active center polyethylene catalyst. By modifying the silica gel with fluorine, the relative molecular weight of the polymer can be improved, and at the same time, the The copolymerization performance of the catalyst, but the effect of improving the polymerization activity is not obvious
[0010] There is no report on the supported chromium vanadium metal oxide double active center ethylene polymerization catalyst co-modified by titanium and fluorine, and the present invention further introduces the modified group Divide titanium and fluorine, improve the copolymerization performance while increasing the catalyst activity, increase the relative molecular weight distribution width of polyethylene products, and improve the performance of polyethylene resin

Method used

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  • Titanium fluoride modified load type chrome alum double-active center catalyst and preparation method thereof
  • Titanium fluoride modified load type chrome alum double-active center catalyst and preparation method thereof
  • Titanium fluoride modified load type chrome alum double-active center catalyst and preparation method thereof

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preparation example Construction

[0126] The preparation methods mentioned in the examples are conventional methods unless otherwise specified. The materials are commercially available unless otherwise specified. The silica gel used in the examples is commercially available Davison955.

[0127] Various polymer properties in the examples were measured according to the following methods:

[0128] High Temperature Gel Chromatography (HT-GPC)

[0129] The weight-average molecular weight and molecular weight distribution of polyethylene products are determined by high-temperature gel chromatography: In this experiment, PL-220 high-temperature gel permeation chromatography (Polymer Laboratories Company) is used to determine the molecular weight of polyethylene and its molecular weight distribution. In the experiment, 1,2,4-trichlorobenzene was used as solvent and measured at 160°C. Data were processed using a universal calibration method using narrow distribution polystyrene as the standard.

[0130] Differentia...

Embodiment 1

[0133] Put 10g of silica gel (pore volume is 1.5 ~ 1.7cm 3 / g, the surface area is 250~300m 2 / g) immersed in a n-hexane solution of tetra-n-butyl titanate (titanium loading: 3wt%), after continuous stirring for 4 hours, dry at 80°C in an oil bath for 4 hours, and then use vacuum drying for 2 hours to further remove the solvent in the silica gel carrier channel , transferred to a blast drying oven at 80°C for 8 hours; then the dried samples were roasted and activated in a fluidized bed, kept at 600°C for 4 hours under high-purity air, and the silica gel was finally cooled down naturally under nitrogen. The above-mentioned roasting procedure is as follows: figure 1 As shown, the titanium dioxide modified silica gel prepared by the impregnation method was obtained. The obtained titanium-modified silica gel was immersed in an aqueous solution of ammonium hexafluorosilicate (the fluorine load was 1.5 wt%). After continuous stirring for 4 hours, dry in an oil bath at 120°C for 6 ...

Embodiment 2

[0135] Put 10g of silica gel (pore volume is 1.5 ~ 1.7cm 3 / g, the surface area is 250~300m 2 / g) immersed in a n-hexane solution of tetra-n-butyl titanate (titanium loading: 3wt%), after continuous stirring for 4 hours, dry at 80°C in an oil bath for 4 hours, and then use vacuum drying for 2 hours to further remove the solvent in the silica gel carrier channel , transferred to a blast drying oven at 80°C for 8 hours; then the dried samples were roasted and activated in a fluidized bed, kept at 600°C for 4 hours under high-purity air, and the silica gel was finally cooled down naturally under nitrogen. The above-mentioned roasting procedure is as follows: figure 1 As shown, the titanium dioxide modified silica gel prepared by the impregnation method was obtained. The obtained titanium-modified silica gel was immersed in an aqueous solution of ammonium hexafluorosilicate (the fluorine load was 1.5 wt%). After continuous stirring for 4 hours, dry in an oil bath at 120°C for 6 ...

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Abstract

The invention belongs to polyethylene catalysts, and particularly relates to a titanium fluoride modified load type chrome alum double-active center catalyst. The titanium fluoride modified load type chrome alum double-active center catalyst comprises an inorganic carrier and loaded active components and modified components. The active components comprise chromium oxides and vanadium oxides, and the modified components comprise fluorine and titanium. According to the catalyst, the content and distribution of comonomers are improved, the number of the comonomers inserted into a low molecular weight end is reduced, the number of the comonomers inserted into a high molecular weight end is increased, and therefore more chalaza molecules can be formed easily, and polyethylene products with better performance are prepared. Meanwhile, the catalyst has the advantages of being high in activity, sensitive in hydrogen regulation response performance and the like. The invention further provides a preparation method of the catalyst. The inorganic carrier is firstly loaded with one of the modified components, and then loaded with the rest of the components, the process is reasonable, and industrial production is easy.

Description

technical field [0001] The invention belongs to a polyethylene catalyst, in particular to a titanium-fluorine-modified supported chromium-vanadium double-active center catalyst and a preparation method thereof. Background technique [0002] Currently known polyethylene catalysts mainly include Ziegler-Natta catalysts, chromium-based catalysts, metallocene catalysts and other non-metallocene catalysts. Among them, chromium-based catalysts are favored by the market for their outstanding contribution to the production of high-density polyethylene and the irreplaceability of their products, and up to now, about 50% of the world's high-density polyethylene is still produced by them. [0003] J.PHogan and R.L.Bank both reported silica gel-loaded chromium oxide catalysts in the patent US2825721, that is, the first-generation Phillips catalysts known later. Some patents such as US4294724, US4295997, US4528338, US5401820, US6388017, etc. have carried out modification research on suc...

Claims

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Application Information

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IPC IPC(8): C08F10/02C08F4/69C08F4/02
CPCY02P20/52
Inventor 李留忠孙巧巧范大鹏程瑞华严婕刘柏平
Owner CHINA PETROLEUM & CHEM CORP
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