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Ethylene/alpha-alkene copolymerization catalyst as well as preparation and application thereof

An olefin copolymerization and catalyst technology, applied in the field of Ziegler-Natta catalysts, can solve the problems of ethylene/1-hexene copolymerization, difficult catalyst solid separation, uneven distribution of 1-hexene, etc., and achieve low cost and good particle shape , The effect of simple preparation process

Active Publication Date: 2014-03-26
PETROCHINA CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The method of ethylene copolymerization disclosed in CN 98101108 is to dissolve magnesium chloride in organic epoxy compounds, organic phosphorus compounds and then add electron donors to form a uniform solution, and then mix with at least one precipitation aid and transition metal titanium halides and derivatives thereof The catalyst is highly active in catalyzing ethylene / 1-hexene copolymerization, and the insertion rate of 1-hexene in the copolymer is relatively high, but the mother liquor of the catalytic system is relatively viscous during the preparation process, and it is difficult to separate the catalyst solid from the mother liquor, and Uneven distribution of 1-hexene in the copolymer
CN11964993 discloses a catalyst for ethylene slurry polymerization, which is dissolved in a homogeneous solution of organic epoxy compound, organic phosphorus compound and inert solvent by magnesium chloride, and then adds electron donor, a kind of co-diluent and transition metal titanium prepared from the chloride of ethylene, this catalyst can also be used for the copolymerization of ethylene and α-olefin, but there is no example of ethylene / 1-hexene copolymerization of LLDPE

Method used

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  • Ethylene/alpha-alkene copolymerization catalyst as well as preparation and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Catalyst 1 is prepared as follows:

[0030] (1) Add 1 g of anhydrous magnesium chloride, 30 ml of n-hexane and 3.75 ml of isobutanol into a three-neck flask replaced by argon, stir and heat to 70° C., and react for 3 hours to obtain a suspension.

[0031] (2) Add 0.05 ml of 2,2-dimethoxypropane to the suspension, stir and react at 70° C. for 1 hour, then add 0.3 ml of tetraethoxysilane, and stir and react at 70° C. for 1 hour.

[0032](3) Cool down to room temperature, slowly add 24 ml of titanium tetrachloride dropwise for 90 minutes; gradually raise the temperature to 70° C. for 2 hours; then stir and react for 2 hours.

[0033] (4) Hydraulically filter the supernatant, add 25 ml of n-hexane, heat up to 70°C, add 0.05 ml of tetraethoxysilane, stir and react for 1 hour; then add 0.025 ml of 2,2-dimethoxypropane, stir and react 1 hour.

[0034] (5) Then add 12 ml of titanium tetrachloride and react for 2 hours. After the reaction, it was washed with n-hexane for seve...

Embodiment 2

[0036] The preparation method of catalyst 2 is the same as embodiment 1, and difference is:

[0037] In step (1), add 35 ml of n-hexane and 2.50 ml of isobutanol to 1 g of anhydrous magnesium chloride, stir and heat to 70° C., and react for 5 hours.

[0038] In step (2), the amount of 2,2-dimethoxypropane is 0.10 ml, and the reaction time is 0.5 hours; the tetraethoxysilane is replaced by cyclohexylmethyldimethoxysilane, and the amount is 0.05 ml, and the reaction time is 2 hours.

[0039] In step (4), the amount of 2,2-dimethoxypropane used is 0.02 ml, and the reaction time is 2 hours.

[0040] The reaction time of titanium tetrachloride in step (5) is 3 hours.

[0041] The titanium content of the obtained solid catalyst 2 was 4.90%.

Embodiment 3

[0043] The preparation method of catalyst 3 is with embodiment 1, difference is:

[0044] In step (1), replace 30 ml of n-hexane with 35 ml of n-heptane, and replace 3.75 ml of isobutanol with 2.50 ml of n-hexanol, stir and heat to 90° C., and the reaction time is 2 hours.

[0045] Replace 2,2-dimethoxypropane with tetrahydrofuran in step (2), its consumption 0.20 milliliters, reaction time 2 hours; Replace tetraethoxysilane with 3-chloropropyl triethoxysilane, its consumption 0.40 milliliters, react Time 0.5 hours.

[0046] In step (3), the amount of titanium tetrachloride is 15 milliliters, the dropwise addition time is 2 hours, the temperature is raised to 90° C., and the reaction time is 1 hour.

[0047] Step (4) heats up to 90°C, replaces tetraethoxysilane with 3-chloropropyltriethoxysilane, the amount is 0.015 ml, and the reaction time is 2 hours; replaces 2,2-dimethoxypropane with tetrahydrofuran, the amount 0.15 ml, reaction time 0.5 hours.

[0048] The amount of ti...

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Abstract

The invention relates to an ethylene / alpha-alkene copolymerization catalyst as well as preparation and application thereof. The ethylene / alpha-alkene copolymerization catalyst is prepared by reacting a magnesium compound, a titanium compound and two electron donors; the electron donor I is an ether compound and comprises tetrahydrofuran, glycol dimethyl ether, 2.2-dimethylpropane and 1,2-dimethoxyethane; the electron donor II is a siloxane compound, the general formula of the siloxane compound is R1xR2ySi(OR3)z, wherein R1 and R2 are respectively alkyl or halogen, R3 is the alkyl, x is more than or equal to 0 and less than 2, y is more than or equal to 0 and less than 2, z is more than 0 and less than or equal to 4; the ethylene / alpha-alkene copolymerization catalyst particularly comprises tetraethoxysilane, 3-chloropropyl triethoxysilane and cyclohexyl dimethoxydimethylsilane. The ethylene / alpha-alkene copolymerization catalyst disclosed by the invention is suitable for catalyzing the ethylene homopolymerization and the ethylene / alpha-alkene copolymerization and the copolymerization of ethylene and long-chain alpha-alkene, such as 1-hexylene, 1-octylene and 1-decene, especially and can be used for preparing the polyalkene with a long branched chain.

Description

technical field [0001] The invention relates to an electron donor-modified Ziegler-Natta catalyst for ethylene / α-olefin copolymerization and its preparation and application. Background technique [0002] Linear low-density polyethylene (LLDPE) is a copolymer of ethylene and α-olefin (ethylene / 1-butene, ethylene / 4-methyl-1-pentene) successfully developed in the 1970s, with a linear molecular structure , the density is 0.910~0.940g / cm 3 . After the introduction of α-olefin monomers into the polymer, the macromolecule contains a considerable amount of branched chains. These short-chained and long-chained branches will affect its physical properties. It can be controlled by adjusting the length of the branched chain, the degree of branching and the content of comonomers. etc. to prepare the desired product. LLDPE combines many advantages of low-density polyethylene and high-density polyethylene, so it has low-temperature toughness, high modulus, bending resistance, puncture r...

Claims

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Application Information

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IPC IPC(8): C08F210/16C08F4/658C08F4/649
CPCC08F210/16
Inventor 陈谦米普科于部伟李群英许胜刘敏李建忠范玲婷王桂芝熊玉洁贺德福徐显明张志高韩云光张爱萍宋春风韩雪梅魏军凤李文鹏史秀娟于杨
Owner PETROCHINA CO LTD
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