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Preparation method of high-isotacticity alloy material

A technology of high-isotactic polybutene and polybutene alloy, which is applied in the production of bulk chemicals and energy input, can solve the problems of not meeting the development prospect of green synthetic chemistry, low polymerization temperature, etc. The effect of uniform diameter distribution and less public works

Active Publication Date: 2017-06-20
QINGDAO UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, considering the polymerization process factors, the polymerization temperature is still low, and at the same time, a large amount of organic solvents still need to be used, and complex processes such as recovery, separation and purification of organic solvents are required, which is not in line with the development prospects of green synthetic chemistry.

Method used

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  • Preparation method of high-isotacticity alloy material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] The entire polymerization system was evacuated and replaced with vacuum nitrogen.

[0042] 1) Propylene prepolymerization:

[0043] The catalyst used is a titanium tetrachloride catalyst supported by magnesium dichloride, wherein the catalyst has a titanium loading amount of 2.8 wt%, and contains 10 wt% of internal electron donor diisobutyl phthalate.

[0044] Polymerization grade liquid phase propylene monomer (feed rate is 1.6kg / hr), triethylaluminum (feed rate is 20g / hr), external electron donor cyclohexylmethyldimethoxysilane (feed rate is 0.8g / hr), hydrogen (feed amount is 22g / hr), main catalyst (feed amount is 2g / hr) enter the high-speed mixer, and the material enters the pipe at a speed of 3L / hr after mixing. A pre-polymerization tubular reactor with a volume of 3 L, a pre-polymerization temperature of 50° C., and a residence time of 1 h. Then the unreacted propylene monomer and hydrogen are separated by a separation device to obtain active polypropylene partic...

Embodiment 2

[0050] The entire polymerization system was evacuated and replaced with vacuum nitrogen.

[0051] 1) Propylene prepolymerization:

[0052] The catalyst used is a titanium tetrachloride catalyst supported by magnesium dichloride, wherein the catalyst has a titanium loading amount of 2.8 wt%, and contains 10 wt% of internal electron donor diisobutyl phthalate.

[0053] Polymerization grade liquid phase propylene monomer (feed amount is 12kg / hr), triethylaluminum (feed amount is 15g / hr), external electron donor dicyclohexyldimethoxysilane (feed amount is 0.4g / hr), the main catalyst (feed rate is 5g / hr) enters the high-speed mixer, and the mixed material enters the prepolymerization tubular reactor that the tube length is 100 meters and the volume is 20L at a speed of 100mL / m, and the prepolymerization temperature is 20L. 90°C, the residence time is 2h. Then the unreacted propylene monomer and hydrogen are separated by a separation device to obtain active polypropylene particle...

Embodiment 3

[0059] The entire polymerization system was evacuated and replaced with vacuum nitrogen.

[0060] 1) Propylene prepolymerization:

[0061] The aluminum alkyl used is diethylaluminum chloride, hydrogen gas (feed rate is 2g / hr), and the prepolymerization temperature is 10°C, and the others are the same as in Example 2.

[0062] 2) Polymerization of butene:

[0063] The polymerization temperature of the tubular reactor is 50°C, the mass ratio of hydrogen to butene is 0.3:100, the polymerization temperature of the horizontal self-cleaning reactor is 50°C, and the others are the same as in Example 2.

[0064] 3) Extrusion:

[0065] 100g anti-aging agent DLTDP, the length-to-diameter ratio of the twin-screw extruder used is 50:1, the extrusion and granulation conditions are: 140°C in zone 1, 160°C in zone 2, 170°C in zone 3, 185°C in zone 4, 190°C in zone 5 , head 190 ℃, rotating speed 10r / min, others are the same as embodiment 2. The experimental results are listed in Table 1. ...

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Abstract

The invention discloses a preparation method of a high-isotacticity alloy material. The method comprises the following steps: 1) carrying out liquid-phase bulk prepolymerization on propylene to generate active high-isotacticity polypropylene granules; 2) recovering the unreacted propylene monomer, and sending the active high-isotacticity polypropylene granules into a tubular reactor to carry out butylene bulk polymerization; 3) sending the material into a horizontal self-cleaning reactor, and further carrying out butylene bulk polymerization to synthesize high-isotacticity polybutylene; 4) terminating the polymerization, and recovering the unreacted butylene monomer; and 5) carrying out further monomer recovery and extrusion granulation on the polymer in an extruder. The method has the advantages of simple technical process, high monomer conversion rate, small occupied space of polymerization equipment, non-sticking polymer, long operating cycle of polymerization equipment and fewer public works. The polybutylene alloy material has the advantages of narrow molecular weight distribution and low volatile content.

Description

technical field [0001] The invention relates to the technical field of preparation of polyolefin materials, in particular to a preparation method of polybutene alloy. Background technique [0002] Isotactic polybutene is a semi-crystalline polymer characterized by high flexibility, outstanding thermal creep resistance, and high tensile strength at elevated temperatures. However, it takes a long time to cool and solidify from the melt, and it often takes more than 7 days to show stable performance. It has been reported (Journal of applied polymer science, 1985, 3163; Journal of Macromolecular Science, Part B, 2012, 926; Macromolecules, 2004, 3755) that it can be physically blended with polyethylene, polypropylene and other polymers or in polymer chains The introduction of ethylene or other α-olefin monomer units can effectively shorten the molding time of polybutene. Since polybutene and polypropylene or polyethylene are thermodynamically incompatible systems, there are two...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L23/20C08L23/12C08L53/00B29C47/92B29C48/92
CPCC08L23/20B29C48/92B29C2948/9258B29C2948/92704C08L2205/03C08L2308/00C08L2314/00C08L23/12C08L53/00Y02P20/52Y02P20/129
Inventor 贺爱华马韵升邵华锋栾波王日国姚刚
Owner QINGDAO UNIV OF SCI & TECH
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