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Spherical polybutylene-1 with high isotacticity and preparation method thereof

A technology of polybutene and isotacticity, which is applied in the field of special catalyst system for dimensional spherical polybutene-1, can solve the problems of complicated production process, production cost, mass transfer, heat transfer difficulty, and reduced production efficiency. Achieving the effect of simple and effective polymerization method

Active Publication Date: 2015-06-03
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Polymerization temperature is higher than 30 o At C, polybutene-1 swells in its monomers, thereby making the system sticky, causing difficulties in mass transfer and heat transfer, which limits the polymerization process to termination at low conversion rates, and reduces production efficiency. At the same time, the complexity of the production process and the increase in production costs

Method used

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  • Spherical polybutylene-1 with high isotacticity and preparation method thereof
  • Spherical polybutylene-1 with high isotacticity and preparation method thereof
  • Spherical polybutylene-1 with high isotacticity and preparation method thereof

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Effect test

Embodiment 1

[0036]After the 1L stainless steel high-pressure polymerization kettle (double-screw stirring paddles) was pumped and replaced several times with high-purity nitrogen, 280 g of butene-1 (Bt) monomer, 9 mmol of triethylaluminum, and 0.1 mmol of ethylene were sequentially added to the reaction kettle Triethoxysilane and 0.0383g heterogeneous Ziegler-Natta catalyst (wherein, the carrier is MgCl 2 , the titanium compound is TiCl 4 ; The mass content of titanium in the catalyst is 2.5%, the internal electron donor is phthalic anhydride (the mass content in the catalyst is 0.3%)), the partial pressure of hydrogen is 0.03MPa, 0°C for 0.5h, and then 35°C Constant temperature polymerization for 3.5h, after the end of the polymerization, flash off the unreacted monomers to directly obtain 120g of spherical polybutene (see figure 1 ), the catalytic efficiency is 125.3Kg polymer / gTi, the bulk density is 0.31 g / cm3, and the melt index is 0.5 g / 10min. The content of insoluble matter obtai...

Embodiment 2

[0038] After the 1L stainless steel high-pressure polymerization kettle (double-screw belt stirring paddle) was exhausted and replaced several times with high-purity nitrogen, 280 g of butene-1 (Bt) monomer, 8 mmol of triethylaluminum, and 0.5 mmol of ethylene were sequentially added to the reaction kettle Trimethoxysilane and 0.0292g heterogeneous Ziegler-Natta catalyst (wherein, the carrier is MgCl 2 , the titanium compound is selected from TiCl4; the mass content of titanium relative to the catalyst is 2.5%, the internal electron donor is phthalic anhydride (the mass content in the catalyst is 1%)), the hydrogen partial pressure is 0.03MPa, and polymerized at 5°C 0.5h, then 3.5h of constant temperature polymerization at 40°C. After the polymerization, the unreacted monomers were flashed to obtain 110g of spherical polybutene directly, with a catalytic efficiency of 150Kg polymer / gTi, a bulk density of 0.35 g / cm3, and a melt index 0.8g / 10min. The content of insoluble matter...

Embodiment 3

[0040] After the 1L stainless steel high-pressure polymerization kettle (double-screw ribbon stirring paddle) was exhausted and replaced with high-purity nitrogen several times, 280 g of butene-1 (Bt) monomer, 7.8 mmol of triethylaluminum, 0.1 mmol of The heterogeneous Ziegler-Natta catalyst of diisobutyldimethoxysilane and 0.0296g (wherein, carrier is MgCl , titanium compound is selected from TiCl 4 ; The mass content of titanium relative to the catalyst is 2.5%, the internal electron donor is diisobutyl phthalate, (the mass content in the catalyst is 2%)), hydrogen partial pressure 0.03MPa, 10 ℃ polymerization 10min, Then 30°C constant temperature polymerization for 3.5h, after the polymerization, the unreacted monomers were flashed off to directly obtain 100g of spherical polybutene (see figure 2 ), the catalytic efficiency is 135Kg polymer / gTi, the bulk density is 0.29g / cm3, and the melt index is 0.75 g / 10min. The content of insoluble matter obtained by extraction with d...

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Abstract

The invention discloses spherical polybutylene-1 with high isotacticity and a preparation method thereof as well as a catalyst used by the method. The method comprises the following steps: catalyzing the polymerization of a butene-1 monomer body to polymerize by using a loaded ziegler-giulio natta spherical catalyst system, wherein hydrogen is a molecular weight adjustor; adding an electron donor compound; implementing temperature-gradient polymerization in a temperature range from -10 DEG C to 50 DEG C, wherein polybutylene-1 suspends in the reaction system in form of spherical particles; and flashing to recover unpolymerized monomers to obtain spherical polybutylene-1. Spherical polybutylene-1 with high isotacticity can be obtained by adjusting the partial pressures of the electron donor and hydrogen, wherein the isotacticity is greater than 95%, the isotacticity is greater than 0.30g / cm<3> and the isotacticity is 0.1-30g / 10min. The catalyst used in the method consists of a carrier, an active component, the electron donor and a promoter.

Description

technical field [0001] The present invention relates to a kind of high isotacticity polybutene-1 polymer and its preparation method and the catalyst used in the method, specifically, the present invention relates to a kind of isotacticity greater than 95%, polybutene in spherical shape The invention relates to ene-1 and its preparation method, and also relates to a special catalyst system for synthesizing high-isotactic spherical polybutene-1. Background technique [0002] High isotactic polybutene-1 has outstanding thermal creep resistance and stress cracking resistance, and has a very high heat distortion temperature, and its service temperature is -20 o C to 105 o C, can be used for a long time at 100 degrees, is an excellent cold and hot water pipe material. [0003] The preparation method of high isotactic polybutene-1 includes solution polymerization, slurry polymerization and gas phase polymerization. U.S. Patent 3,944,529, 5,237,013, and 6,306,996 all adopt soluti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F110/08C08F4/649C08F4/02C08L23/20
Inventor 贺爱华王超
Owner QINGDAO UNIV OF SCI & TECH
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