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[N,P] type all-heterocyclic non-metallocene catalyst, preparation method and applications thereof

A catalyst and main catalyst technology, applied in the field of olefin polymerization catalyst and olefin coordination polymerization, can solve the problems of non-metallocene catalyst ligand structure design and large variability in synthesis

Pending Publication Date: 2020-03-31
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the design and synthesis of the ligand structure of non-metallocene catalysts are highly variable

Method used

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  • [N,P] type all-heterocyclic non-metallocene catalyst, preparation method and applications thereof
  • [N,P] type all-heterocyclic non-metallocene catalyst, preparation method and applications thereof
  • [N,P] type all-heterocyclic non-metallocene catalyst, preparation method and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] (1) Synthesis of catalyst compound 1 meeting general formula (1)

[0055] Take 50ml of toluene, 12ml (0.1314mol) of aniline, 21.4ml (0.0657mol) of diphenylsilylform, and 0.1314mol of phenylphosphine chloride in a 300ml schlenk bottle, heat it to 45°C and react for 4h, drain it, and pour it into the remaining 100ml of n-hexane was added to the solid, dissolved and filtered, and the filtrate was recrystallized to obtain 11.4g of anilinophenylphosphine silane, yield: 61%.

[0056] (2) Preparation of main catalyst compound 1

[0057] Under the protection of nitrogen, 0.43 g of compound 2-1 conforming to the general formula (2) was dissolved in 30 mL of toluene, and then 0.11 mL (1 mmol) of titanium tetrachloride was added, and the temperature was raised to 55° C. for 5 h of reaction. The solvent was removed in vacuo, and the residue was washed 3 times with n-hexane and dried to obtain 0.53 g of compound 1 (Cat. 1) conforming to the general formula (1). 1 H NMR (600MHz, CD...

Embodiment 2

[0063] (1) Preparation of main catalyst compound 2:

[0064] According to the method of Example 1, the solvent is changed to n-heptane, and 0.43g of compound 2-2 conforming to the general formula (2) is weighed to react with 0.23g (1mmol) zirconium tetrachloride to obtain 0.45g conforming to the general formula (1) Compound 2 (Cat.2). 1 H NMR (600MHz, CDCl 3 ): δ7.46(4H, m), δ7.38(2H, t), δ7.05-7.14(10H, m), δ6.67-6.95(4H, m), δ6.67(2H, t) , δ6.55(2H,d), δ0.67(6H,s); Anal.Calcd.(%) for C 22 h 24 NPOSiZrCl 2 : C:48.79, H:4.48, N:2.60; found: C:49.03, H:4.52, N:2.53.

[0065] (2) Propylene polymerization:

[0066] Under anhydrous and oxygen-free conditions, 9 mg of the main catalyst, 100 ml of toluene, and 3 ml of triethylaluminum solution (1M) were sequentially added into a 300 ml reaction flask. The air was changed three times, the temperature was raised to 40° C., the pressure of propylene was 2.5 MPa, and the polymerization was carried out for 100 minutes. The reacti...

Embodiment 3

[0070] (1) Preparation of main catalyst compound 3:

[0071] According to the method of Example 1, 0.45 g of compound 2-23 conforming to general formula (2) was reacted with 0.21 g (1 mmol) of yttrium trichloride to obtain 0.36 g of compound 3 (Cat.3) conforming to general formula (1). 1 H NMR (600MHz, CDCl 3 ): δ3.44(4H, m), δ2.36(2H, t), δ2.05-2.18(10H, m), δ2.68-2.96(4H, m), δ2.68(10H, t) , δ2.56(3H, d), δ0.97(3H, s); Anal.Calcd.(%) for C 19 h 36 NPOSiYCl: C, 44.45; H, 7.07; N, 2.73; found: C, 44.35; H, 6.99; N, 2.79.

[0072] (2) Ethylene polymerization:

[0073] Under anhydrous and oxygen-free conditions, 6 mg of main catalyst, 100 ml of toluene, and 7 ml of MAO solution (10 wt %) were successively added into a 300 ml reaction flask. The air was changed three times, the temperature was raised to 90°C, the ethylene pressure was 0.8 MPa, and the polymerization was carried out for 90 minutes. The reaction was terminated with ethanol solution containing 10% hydrochloric...

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Abstract

The invention provides a [N,P] type all-heterocyclic non-metallocene catalyst, a preparation method and applications thereof. The preparation method comprises the following steps: providing a compoundrepresented by a general formula (1), wherein in the general formula (1), R1 and R2 are respectively and independently selected from C1-C20 alkyl, C1-C20 alkoxy, C3-C20 cycloalkyl, C3-C20 cycloalkyloxy, C6-C20 aryl and C6-C20 phenolic aryl, R3 and R4 are respectively and independently selected from a hydrogen atom, C1-C20 alkyl, C3-C20 cycloalkyl, and C6-C20 aryl, Xis selected from H, F, Cl, Br,I and C1-C20 alkyl, and M represents a transition metal atom and is selected from IIIB group element, IVB group element, VB group element and VIII group element. The compound provided by the inventioncan be used as a main catalyst of an olefin polymerization catalyst. The invention also provides an olefin polymerization catalyst containing the compound represented by the general formula (1), a preparation method and applications thereof.

Description

technical field [0001] The invention belongs to the field of olefin polymerization catalysts and olefin coordination polymerization, in particular to [N,P] type non-metallocene catalysts for ethylene or propylene homopolymerization, ethylene / α-olefin copolymerization or propylene / α-olefin copolymerization and application. Background technique [0002] Non-metallocene catalysts have received extensive attention because of their single active center, catalyst activity, polymer stereoregularity, molecular weight and molecular weight distribution can be controlled by changing the ligand structure; and the polymers synthesized by non-metallocene catalysts The excellent performance has been unanimously recognized. [0003] Polyolefin products have many advantages, such as easy processing, good thermal stability, good weather resistance, good chemical corrosion resistance and long service life, etc., and are very popular in the market. However, polyolefins (such as PE, PP, etc.) ...

Claims

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Application Information

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IPC IPC(8): C07F5/06C07F7/00C07F9/6596C07F15/00C07F15/04C07F15/06C07F5/00C08F10/02C08F10/06C08F4/642
CPCC07F9/6596C07F5/003C07F15/008C07F15/045C07F15/065C07F15/0066C07F5/069C08F10/02C08F10/06C08F4/6428
Inventor 王科峰黄启谷义建军李荣波许蔷王东明曾令志王静王帆雷珺宇
Owner PETROCHINA CO LTD
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