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Core-shell type spherical metallocene ethylene propylene rubber and preparation method thereof

A technology of ethylene-propylene rubber and metallocene, which is applied in the field of core-shell spherical metallocene ethylene-propylene rubber and its preparation, which can solve the problems of short production process, no outstanding advantages in product performance, and narrow application range, and achieve high-efficiency ethylene-propylene rubber. Rubber content, achieve solvent-free discharge, prevent sticking and clumping effect

Inactive Publication Date: 2014-10-01
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, its mature technology, good product comprehensive performance, fast vulcanization speed, and wide range of product applications are still the most widely used method for producing ethylene-propylene rubber at home and abroad. In addition, the catalyst has low catalytic efficiency and needs to be washed and removed.
The investment and cost process of the suspension polymerization process is respectively equivalent to 77% and 88% of the solution polymerization process of the same scale. It has the characteristics of short production process, less investment, low raw material consumption and energy consumption, low production cost, and less three waste treatment costs. However, the product performance has no outstanding advantages, and the application range is narrow
Gas-phase polymerization process products contain a large amount of carbon black, which is poor in versatility and limits its scope of use. However, its short process flow, efficient and clean production are conducive to reducing production costs and environmental protection. The investment and product costs are the lowest, respectively equivalent to 42% and 68% of the same scale solution polymerization process

Method used

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  • Core-shell type spherical metallocene ethylene propylene rubber and preparation method thereof
  • Core-shell type spherical metallocene ethylene propylene rubber and preparation method thereof
  • Core-shell type spherical metallocene ethylene propylene rubber and preparation method thereof

Examples

Experimental program
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Effect test

preparation example 1

[0037] Preparation Example 1 Preparation of Hollow Polyethylene Spherical Particle 1

[0038] Before the experiment, the stainless steel Büchi autoclave was baked with an electric gun for 3 minutes, pumped three times with high-purity nitrogen, and finally placed in a nitrogen atmosphere, turned on mechanical stirring, and added 100 mL of n-heptane through the feeding port, and then three Ethyl aluminum (TEA, 1mol / L), and finally wash down 4 mg of the main catalyst with 100 mL of n-heptane, close the feeding port, and feed propylene to start prepolymerization. The molar ratio of aluminum in the cocatalyst to titanium in the main catalyst is 120, and the main component of the main catalyst is: TiCl 4 , MgCl 2 , and diisobutyl phthalate, are spherical particles with a particle size of 30-50 microns. Its titanium content is 2.7 wt%. The reaction conditions of the pre-polymerization are: the pressure is 0.1 MPa, the temperature is 10° C., and the time is 2 min. After the prepo...

preparation example 2

[0040] Preparation Example 2 Preparation of Hollow Polyethylene Spherical Particles 2

[0041] Preparation Example 1 was basically repeated, except that the prepolymerization reaction temperature was 30° C., the prepolymerization time was 20 minutes, and the amount of propylene added was 10 mmol. The hydrogen gas is 50 mL, the ethylene polymerization pressure is 0.9 MPa, the ethylene polymerization temperature is 40° C., and the ethylene polymerization time is 20 minutes.

[0042] The obtained hollow polyethylene spheres had a weight average molecular weight of 1200 kg / mol, a molecular weight distribution index of 6, a melting point of 125° C. and a porosity of 0.60 mL / g.

preparation example 3

[0043] Preparation Example 3 Preparation of Hollow Polyethylene Spherical Particles 3

[0044] Preparation Example 1 was basically repeated, except that the prepolymerization reaction temperature was 50° C., the prepolymerization time was 25 minutes, and the amount of propylene added was 30 mmol. The hydrogen gas is 70mL, the ethylene polymerization pressure is 0.4MPa, the ethylene polymerization temperature is 50°C, and the ethylene polymerization time is 60min.

[0045] The obtained hollow polyethylene sphere had a weight average molecular weight of 900 kg / mol, a molecular weight distribution index of 7, a melting point of 130° C. and a porosity of 0.72 mL / g.

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Abstract

The invention relates to the field of metallocene ethylene propylene rubber and aims to provide a core-shell type spherical metallocene ethylene propylene rubber and a preparation method thereof. The core-shell type spherical metallocene ethylene propylene rubber comprises a core and a shell layer with a hollow structure, wherein the shell layer is made of polyethylene, and the core is made of ethylene-propylene random copolymer. The preparation method comprises the following steps of: preparing polyethylene spherical particles, preparing metallocene-supported polyethylene particles by using the polyethylene spherical particles, and then preparing the core-shell type spherical metallocene ethylene propylene rubber through carrying out a copolymerization reaction on the polyethylene spherical particles. The core-shell type spherical metallocene ethylene propylene rubber disclosed by the invention is high in ethylene propylene rubber content and capable of effectively preventing the sticking and aggregation of the polymer particles in vapour phase polymerization, thus realizing solvent-free discharge during an ethylene propylene rubber preparation process.

Description

technical field [0001] The invention relates to the field of preparation of metallocene ethylene propylene rubber, in particular to a core-shell spherical metallocene ethylene propylene rubber and a preparation method thereof. Background technique [0002] Ethylene-propylene rubber (EPR) is a kind of copolymerized rubber with ethylene and propylene as basic monomers that came out after the invention of Zieg1er-Natta catalyst and the appearance of polyethylene and polypropylene. It is divided into binary ethylene-propylene rubber (EPR) and There are two types of ethylene propylene diene monomer (EPDM). The former is a copolymer of ethylene and propylene, which was first publicly reported by Natta (a random copolymer of ethylene and propylene); the latter is a copolymer of ethylene, propylene and a small amount of non-conjugated diene. EPR has many excellent properties that other general-purpose synthetic rubbers do not have. In addition, the monomer is cheap and easy to get,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F210/16C08F110/02C08F4/6592C08F4/649C08F4/646C08F4/02C08J9/26
Inventor 傅智盛齐美洲范志强徐涛
Owner ZHEJIANG UNIV