Two-stage material-feeding random gradually-varied butylbenzene co-polymer and preparation method thereof

A styrene-butadiene copolymer and gradient copolymerization technology, applied in the field of random gradient styrene-butadiene copolymer and its preparation, can solve the problems of difficulty in alternating control, complicated process, long feeding time, etc., and achieve better toughening effect and preparation Simple method and increased toughening effect

Active Publication Date: 2015-01-21
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention aims at the defects that the preparation method of the polymer containing the graded styrene-butadiene polymer structure in the prior art has long feeding time, difficulty in realizing alternate control, and complicated process. The second purpose is to provide a process The method for preparing the above-mentioned two-stage feed-containing random gradient styrene-butadiene copolymer is simple, easy to control, and under mild conditions, and the method is easy to realize industrial production

Method used

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  • Two-stage material-feeding random gradually-varied butylbenzene co-polymer and preparation method thereof
  • Two-stage material-feeding random gradually-varied butylbenzene co-polymer and preparation method thereof
  • Two-stage material-feeding random gradually-varied butylbenzene co-polymer and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0040] In a 5L jacketed stainless steel polymerization kettle replaced with nitrogen, introduce 2500mL of purified cyclohexane, add 0.39gTHF and 4mmol of n-butyllithium and stir, heat up to 70-80°C with jacketed hot water, and mix for 22.5 g styrene and 225g butadiene are evenly distributed, and the feeding time is controlled to be 20min. They are added to the polymerization kettle at a uniform speed for the first stage of polymerization until the monomer reaction is complete, and then 52.5g of styrene is added for the second stage of polymerization until the monomer is reacted. complete, 0.18 g of ethanol was added to terminate the polymerization reaction. Put the glue out of the polymerization kettle, add 0.75g of antioxidant 1076 and 0.75g of antioxidant 168, stir evenly, and conduct drying treatment after water precipitation and coagulation to obtain dry polymer glue. GPC chromatographic test obtains that the number-average molecular weight of this polymer is 75000, and th...

Embodiment 2

[0047] In a 5L jacketed stainless steel polymerization kettle replaced with nitrogen, introduce 2500mL of purified cyclohexane, add 0.39g THF and 2mmol n-butyllithium and stir, heat up to 70-80°C with jacketed hot water, and Mix 30.0g styrene and 195g butadiene monomer evenly, control the feeding time at 25 minutes, carry out the first stage of polymerization reaction until the monomer reaction is complete, then add 75.0g styrene polymerization, until the monomer reaction is complete, add 0.09g Ethanol terminates the polymerization reaction. Put the glue out of the polymerization kettle, add 0.75g of antioxidant 1076 and 0.75g of antioxidant 168, stir evenly, and conduct drying treatment after water precipitation and coagulation to obtain dry polymer glue. The number-average molecular weight of the polymer is 150,000, the content of polymer block styrene is 25.0% of the total weight ratio of monomers, the content of mixed styrene in butadiene is 10.0% of the total weight ratio...

Embodiment 3

[0063] In a 5L jacketed stainless steel polymerization kettle replaced with nitrogen, introduce 2500mL of purified cyclohexane, add 0.39g THF and 1mmol n-butyllithium and stir, heat up to 70-80°C with jacketed hot water, and Mix 30.0g styrene and 195g butadiene monomer evenly, control the feeding time at 25 minutes, carry out the first stage of polymerization reaction until the monomer reaction is complete, then add 75.0g styrene polymerization, until the monomer reaction is complete, add 0.09g Ethanol terminates the polymerization reaction. Put the glue out of the polymerization kettle, add 0.75g of antioxidant 1076 and 0.75g of antioxidant 168, stir evenly, and conduct drying treatment after water precipitation and coagulation to obtain dry polymer glue. The number-average molecular weight of the polymer is 300,000, the content of polymer block styrene is 35.0% of the total weight ratio of monomers, the content of mixed styrene in butadiene is 10.0% of the total weight ratio...

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Abstract

The invention discloses a two-stage material-feeding random gradually-varied butylbenzene co-polymer and a preparation method thereof. The co-polymer includes a butylbenzene random gradually-varied co-copolymerized segment and a polystyrene homo-polymerized segment. The preparation method includes following steps: controlling temperature of a reactor being filled with a non-polar hydrocarbon solvent, an activity regulating agent and an initiator; adding a mixed monomer including styrene and butadiene; carrying out a first-stage random polymerization reaction; adding styrene for carrying a further reaction; and adding a terminator for stopping the reactor after the reacting completed. The preparation method is simple in process, is easy to carry out and is mild in reaction conditions. The random gradually-varied butylbenzene co-polymer, when being used for modifying ABS resin, has an excellent toughening effect, a good mechanical performance and an excellent glossiness.

Description

technical field [0001] The invention relates to a random gradient styrene-butadiene copolymer and a preparation method thereof, belonging to the field of styrene-butadiene rubber synthesis. Background technique [0002] The styrene-butadiene polymer structures that have been found include block, tapered and random structures. There are many patent documents related to reported styrene-butadiene block polymers, such as EP0492490, US4925899, US5130377, CN85100418 and so on. With the improvement of polymer performance requirements, inventors have designed various structures. Japanese Patent Laid-Open Application 52-58788 (corresponding to U.S. Patent 4,167,545) discloses branched block copolymers prepared by distributive addition of a catalyst to a block polymerization system. CN1241582A and WO96 / 25442 disclose the preparation method of styrene-butadiene polymer containing tapered segments. The formation of the gradual transition section is obtained by prolonging the feeding...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F297/04C08L53/02C08L55/02
Inventor 陈移姣宋丽莉李望明黄丽芳蒋文英燕富成
Owner CHINA PETROLEUM & CHEM CORP
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