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Preparation method of gas-phase high-impact polypropylene instead of low-purity nitrogen

A technology of high-impact polypropylene and gas-phase method, which is applied in the field of preparation of high-impact polypropylene by gas-phase method, which can solve the problems of low catalyst activity and low ethylene content, and achieve strong dispersion, improved impact strength, and continuous stability The effect of production

Active Publication Date: 2019-08-06
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this prior art is that the activity of the catalyst is low and the ethylene content in the obtained high impact polypropylene is low

Method used

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  • Preparation method of gas-phase high-impact polypropylene instead of low-purity nitrogen
  • Preparation method of gas-phase high-impact polypropylene instead of low-purity nitrogen
  • Preparation method of gas-phase high-impact polypropylene instead of low-purity nitrogen

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Embodiment 1, a kind of preparation method of gas-phase process high-impact polypropylene that replaces low-purity nitrogen, the following steps are carried out in sequence:

[0046] (1) Homopolymerization of propylene:

[0047] The supported Ziegler-Natta catalytic system consists of MgCl 2 / TiCl 4 Type catalyst 2.3g and particle diameter are 50nm superfine titanium dioxide 30mg composition; The MgCl 2 / TiCl 4 The catalyst is based on (9,9-bis(methylmethoxy)fluorene as the internal electron donor, MgCl 2 As a carrier, loading TiCl 4 the catalyst;

[0048] MgCl 2 / TiCl 4 The specific preparation method of the type catalyst is: 4.8g (0.05mol) of anhydrous MgCl 2 After adding 0.025mol 9,9-bis(methylmethoxy)fluorene under the protection of nitrogen, it was immersed in a solution containing 0.48g (2.5mmol) TiCl 4 hexane solution (about 10ml), followed by filtration drying (drying at 60°C for 120 minutes) to give MgCl 2 / TiCl 4 type catalyst.

[0049] The prepara...

Embodiment 2

[0055] Embodiment 2, a method for preparing high-impact polypropylene by gas phase method instead of low-purity nitrogen, the following steps are carried out in sequence:

[0056] (1) Homopolymerization of propylene:

[0057] The supported Ziegler-Natta catalytic system consists of MgCl 2 / TiCl 4 Type catalyst 1.8g and particle diameter are 20nm superfine calcium carbonate 18mg composition; The MgCl 2 / TiCl 4 The type catalyst uses 9,9-bis(benzylcarboxymethyl)fluorene as the internal electron donor, MgCl 2 / TiCl 4 as a carrier catalyst;

[0058] MgCl 2 / TiCl 4 The specific preparation method of the type catalyst is: 9.5g (0.1mol) anhydrous MgCl 2 After adding 0.15mol 9,9-bis(benzylcarboxymethyl)fluorene under the protection of nitrogen, it was immersed in a solution containing 1.9g (9.9mmol) TiCl 4 hexane solution (about 20ml), followed by filtration and drying to obtain MgCl 2 / TiCl 4 type catalyst.

[0059] The preparation method of the supported Ziegler-Natta ca...

Embodiment 3

[0065] Embodiment 3, a method for preparing high-impact polypropylene by gas-phase process instead of low-purity nitrogen, the following steps are carried out in sequence:

[0066] (1) Homopolymerization of propylene:

[0067] The supported Ziegler-Natta catalytic system consists of MgCl 2 / TiCl 4 Type catalyst 3.1g and particle diameter are the superfine silica 0.31g composition of 10nm; The MgCl 2 / TiCl 4 The catalyst is di-n-butyl phthalate as internal electron donor, MgCl 2 / TiCl 4 as a carrier catalyst;

[0068] MgCl 2 / TiCl 4 The specific preparation method of the type catalyst is: 9.5g (0.1mol) anhydrous MgCl 2 Add 0.13 mol of di-n-butyl phthalate under the protection of nitrogen without water, and then impregnate in a solution containing 0.5 g (2.6 mmol) of TiCl 4 hexane solution (about 10ml), followed by filtration and drying to obtain MgCl 2 / TiCl 4type catalyst.

[0069] The preparation method of the supported Ziegler-Natta catalytic system is: adding th...

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Abstract

The invention discloses a preparation method of gas-phase-method high impact polypropylene capable of replacing low-purity nitrogen. The preparation method comprises the following steps: performing polymerization in a polymerizing kettle with propylene as a monomer and hydrogen as a molecular weight modifier under action of a load type Ziegler-Natta catalyzing system, wherein the load type Ziegler-Natta catalyzing system is prepared from a MgCl2 / TiCl4 type catalyst and inorganic powder I, and the MgCl2 / TiCl4 type catalyst is a catalyst with a bisether or diester compound as an internal electron donor and MgCl2 as a carrier and loads TiCl4; exhausting out gas in the polymerizing kettle after the propylene homopolymerization reaction is finished, then sending propylene-ethylene mixed gas into the polymerizing kettle and adding inorganic powder II to perform propylene ethylene gas-phase copolymerization to obtain high impact polypropylene serving as a product.

Description

technical field [0001] The invention relates to a method for preparing impact-resistant polypropylene, in particular to a method for preparing high-impact polypropylene by gas-phase process instead of low-purity nitrogen. Background technique [0002] Impact polypropylene alloys are a class of high-performance polypropylene resins that are widely used and have significantly higher toughness than conventional homopolypropylene resins. This type of resin is usually prepared by two-stage series polymerization, that is, liquid-phase or gas-phase bulk polymerization of propylene in the first stage, and then transferred to the second stage for ethylene-propylene gas-phase copolymerization. The polypropylene resin obtained through this two-stage polymerization reaction is an in-situ multi-phase polymer material composed of a continuous phase of polypropylene and a dispersed phase of ethylene-propylene copolymer, or a polymer alloy. In the polypropylene alloy, the ethylene-propylen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F10/06C08F110/06C08F210/16C08F210/06C08F4/02C08F4/642C08F4/649C08F2/44
CPCC08F10/06C08F110/06C08F210/16C08F210/06C08F4/022C08F4/6421C08F4/6494C08F2/44
Inventor 姚臻曹堃付强张景陈薇屠宇侠肖智贤马达锋
Owner ZHEJIANG UNIV
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