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Preparation method of polyolefin alloy

A technology of polyolefin and alloy, applied in the field of preparation of polyolefin alloy, can solve the problem that the gas phase preparation of polybutene alloy material is not mentioned in the literature, etc.

Active Publication Date: 2015-07-08
QINGDAO UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Such as Chinese patent (CN102030841, CN102050892 A, CN1516707A, CN101268104A, CN11265478A, CN101016346A, CN10321439A) etc. are all polyethylene, polypropylene gas phase polymerization method, but also there is no document mentioning for the gas phase preparation of high stereoregularity polybutene alloy material

Method used

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  • Preparation method of polyolefin alloy

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Experimental program
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Effect test

Embodiment 1

[0051] Preparation of Polybutene Alloy Materials by Continuous Process

[0052] The gas-phase continuous polymerization preparation method of the polybutene alloy material of the present invention is carried out in the following steps on a set of continuously operating pilot plant:

[0053] Prepolymerization is to carry out in a 5L autoclave full of still operation, loaded titanium catalyst feed rate 2g / h (titanium content 2.5-3.5wt%), co-catalyst triethylaluminum feed rate 6g / h (mixed into 5wt% % hexane solution feeding), the external electron donor diphenyldimethoxysilane, the feeding amount is 0.6g / h, the pre-polymerization feeding amount of propylene is 15kg / h, and the feeding is cooled to 5°C. The prepolymerization temperature was 16°C, and the residence time was 20 minutes to obtain an active prepolymer.

[0054] The gas phase polymerization reaction is carried out in two stages. The volume of the two gas phase reactors is 175L. The active prepolymer enters the first st...

Embodiment 2

[0057] Preparation of Polybutene Alloy Materials by Continuous Process

[0058] Adopt the same continuous polymerization device and operating process as in Example 1, the cocatalyst is changed into triisobutylaluminum, the feed rate is 4g / h (being mixed with the hexane solution feed of 5wt%), and the external electron donor is changed into For diisopropyldimethoxysilane, the pre-polymerization monomer is changed to liquid-phase propylene feed rate to 0.5g / h, and the pre-polymerization time is changed to 1h. Others are the same as embodiment 1.

[0059] The final product obtained is a fine powder spherical particle, and the properties of the polybutene alloy are shown in Table 1.

Embodiment 3

[0061] Preparation of Polybutene Alloy Materials by Continuous Process

[0062] The same continuous polymerization apparatus as in Example 1 was used. Prepolymerization is carried out in a 5L autoclave full of still operation, catalyst active component feed rate 2g / h, cocatalyst triethylaluminum feed rate 6g / h (mixed with 5wt% hexane solution feed) , external electron donor diphenyldimethoxysilane, feed amount 0.6g / h, butene-1 feed amount 16kg / h for prepolymerization, prepolymerization temperature 5°C, residence time 30min to obtain active polymer.

[0063] The gas-phase polymerization reaction is carried out in two stages. The volume of the two gas-phase reactors is 175L. The active prepolymer enters the first-stage reactor, and the mixed gas of butene-1 and hydrogen is pressed into the gas-phase polymerization. Butene-1 1 The gas phase composition is 95mol%, the hydrogen gas phase composition is 5mol%, the polymerization pressure is 0.9MPa, the polymerization temperature is...

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Abstract

The invention discloses a gas-phase bulk polymerization method of a polyolefin alloy, in particular a polybutene alloy material. The method is characterized by (1) adopting a continuous or batch polymerization process; (2) performing gas phase polymerization of the polybutene alloy material in a single gas phase reactor or two or more gas phase reactors which are connected in series; and (3) respectively implementing homopolymerization of two monomers in two stages. The method adopts a single heterogeneous Ziegler-Natta catalyst which has multiple active centers and good hydrogen sensitivity to catalyze stage-by-stage polymerization of butene-1 and propylene, so that the polybutene alloy material which is less in catalyst residue and good in particle shape, does not have agglomerates and has a core-shell structure can be obtained. The prepared polybutene alloy material comprises the following components in percentage by mass: 10-99% of polybutene-1, 1-80% of polypropylene and 0.01-10% of butene-1-propylene copolymer, and can be used for replacing part of polyethylene and polypropylene in use.

Description

technical field [0001] The invention relates to the technical field of preparation of polyolefin alloys, in particular to a bulk gas phase polymerization method of polybutene alloys. Background technique [0002] Polybutene alloy material can shorten the molding cycle without affecting the high temperature creep resistance and impact resistance of polybutene-1 resin, and has the advantages of high modulus, high hardness and rapid setting of polypropylene. [0003] The polybutene alloy prepared by the in-situ polymerization method in the kettle can effectively improve the two-phase dispersion problem. At the same time, the in-situ synthesis of a small amount of copolymer can significantly improve the phase interface problem of the alloy, and the alloy can also be adjusted by changing the polymerization process parameters. Parameters such as component content, molecular weight and its distribution. Therefore, the preparation of polybutene alloy by in-situ polymerization in th...

Claims

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Application Information

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IPC IPC(8): C08L23/12C08L23/20C08F110/06C08F110/08C08F4/649C08F2/34C08F2/01
CPCC08F2/01C08F2/34C08F4/649C08F110/06C08F110/08C08L23/12C08L23/20C08L2205/02
Inventor 贺爱华刘晨光邵华锋姜秀波
Owner QINGDAO UNIV OF SCI & TECH
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