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High isotactic polypropylene alloy material and preparation method thereof

An alloy material and polyolefin technology, which is used in the preparation of regular polyolefin alloy materials and the field of polybutene polypropylene alloy materials, can solve the problems of inability to achieve results, reduced catalytic activity, and uneven distribution of copolymers.

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

AI Technical Summary

Problems solved by technology

However, through the existing technology, it is found that although the rigidity and toughness of the material are balanced to a certain extent, the effect is not particularly obvious. The reason may be that the two-stage method causes uneven distribution of the copolymer and cannot achieve the best effect. At the same time Catalytic activity is also reduced

Method used

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  • High isotactic polypropylene alloy material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0070] 1L full-sealed magnetic stirring stainless steel pressure polymerization kettle, pumped and replaced with high-purity nitrogen for several times, then metered and added triethylaluminum (Al), 100mL of hexane, and external electron donor diphenyl dimethoxide into the reaction kettle Silane (Si) and MgCl 2 Loaded TiCl 4 Catalyst (Ti content 2.5wt.%) 0.25g, add propylene 0.06Kg, wherein Al / Ti=50 (molar ratio), Al / Si=10 (molar ratio). Stir and polymerize at 0°C for 5 minutes, then raise the temperature and depressurize to evacuate propylene and hexane, flush it into a new reactor with inert gas, replace the inert gas with propylene to a pressure of 0.1MPa, and then add 0.01MPa of hydrogen at 30°C React for 6 minutes, then evacuate propylene and hydrogen, add 0.2Kg butene-1, react at 60°C for 1 hour, evacuate butene-1, further feed propylene to a pressure of 0.2MPa, maintain 6 minutes, then evacuate propylene, add 0.2 Kg of butene-1 and 0.01MPa hydrogen were reacted for 1 ...

Embodiment 2

[0072] 1L fully-closed magnetic stirring gas-phase stainless steel pressure polymerization kettle, pumped and replaced with high-purity nitrogen for several times, then metered triethylaluminum (Al), external electron donor cyclohexyltrimethoxysilane (Si) and MgI 2 Loaded TiCl 4 Catalyst (Ti content 2.5wt.%) 0.25g, add propylene 0.05Kg, hydrogen 0.02Mpa, wherein Al / Ti=80 (molar ratio), Al / Si=20 (molar ratio). Stir and polymerize at 0°C for 5 minutes, then heat up and evacuate propylene and hydrogen under reduced pressure, add 0.2Kg of butene-1, react at 55°C for 0.5h, empty butene-1, and feed 0.2MPa of propylene and 0.02 MPa of hydrogen was reacted at 60°C for 10 minutes, then the propylene and hydrogen were evacuated, 0.2Kg of butene-1 was added, and the reaction was carried out at 55°C for 0.5h, and the cycle was repeated three times. After the drying was terminated, 380g of powdered polymer was directly obtained. The properties of the alloy are shown in Table 1.

Embodiment 3

[0074] 10L fully-closed loop reactor, pumped out and replaced with high-purity nitrogen several times, then metered 150ml of heptane, triethylaluminum (AlEt3), and external electron donor diphenyldimethoxysilane into the reactor (Si) and SiO 2 Load VlCl 3 Catalyst (V content 3.3wt.%) 1.0g, add propylene 0.05Kg, wherein Al / V=50 (molar ratio), Al / Si=20 (molar ratio), 0 ℃ of stirring polymerization 1min, then heat up and depressurize discharge Empty propylene and hexane, feed 0.3MPa propylene and 0.03MPa hydrogen into the reactor, react at 60°C for 10 minutes, then empty the propylene and hydrogen, add 0.5Kg of butene-1, react at 35°C for 0.6h, and empty Butene-1, further feed propylene and hydrogen to a pressure of 0.2MPa, maintain for 10min, then empty the propylene, add 0.5Kg of butene-1, react for 0.5h, and cycle like this 4 times, and obtain powder directly after drying Polymer 2.77Kg. The properties of polybutene alloy are shown in Table 1.

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Abstract

The invention discloses a high isotactic polypropylene alloy material and a preparation method thereof. The material contains 5-98.9 parts by weight of polybutylene, 1-80 parts by weight of polypropylene and 0.1-15 parts by weight of propylene-butene copolymer; the isotacticity of the high isotactic polypropylene is larger than 85%, and the smelting point of the high isotatic polypropylene is 115-129 DEG C; the isotacticity of the high isotactic polypropylene is larger than 85%, and the smelting point of the high isotactic polypropylene is 155-169 DEG C; the propylene-butene copolymer contains a random copolymer and a segmented copolymer of propylene-butene. The preparation method uses a titanium / vanadium supported catalyst and adopts a multistage sequential polymerization manner and specifically comprises the steps of carrying out propylene polymerization or butane-1 polymerization, then initiating butane-1 polymerization or propylene polymerization, and respectively carrying out propylene polymerization or butane-1 polymerization, and so on to synthesize the high isotactic polypropylene alloy material. The material is a powdery or spherical product, and has the advantages of excellent impact resistance, thermal creep resistance and low shrinking percentage of polybutylene, high modulus, high surface hardness and fast setting of polypropylene, and the like.

Description

technical field [0001] The invention relates to the field of a novel polyolefin material, in particular to a method for preparing a high-isotactic polyolefin alloy material and a polybutene-polypropylene alloy material prepared by the method. Background technique [0002] Isotactic polybutene has outstanding creep resistance and stress crack resistance, and is an excellent resin for hot water pipes. However, isotactic polybutene has a very slow crystal transformation, and it often takes several days to more than ten days to complete the transformation and present stable performance. Polypropylene has good processability, excellent tensile strength, yield strength, surface hardness and elastic modulus, but lacks toughness and is prone to brittle cracking at low temperatures. [0003] Qingdao University of Science and Technology (Chinese patent ZL 200710013587.X) reported a new polymerization process for the synthesis of polybutene (butene homopolymer) by bulk precipitation p...

Claims

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Application Information

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IPC IPC(8): C08L23/20C08L23/12C08L23/14C08L53/00C08F293/00C08F110/06C08F110/08C08F210/06C08F210/08C08F4/646C08F2/34C08F2/01
CPCC08F210/08C08L23/12C08L23/20C08F2400/02C08L2205/03C08L2314/02C08L23/14C08F210/06C08F4/6465C08F2/34C08F2/01
Inventor 贺爱华姜秀波刘晨光邵华锋
Owner QINGDAO UNIV OF SCI & TECH
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