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H-shaped polymer and preparation method thereof

A technology of polymers and prepolymers, applied in the field of polymers, can solve problems such as low molecular weight of arm chains and poor controllability

Active Publication Date: 2018-06-19
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a new method for preparing H-type polymers in order to overcome the disadvantages of poor controllability or low molecular weight of the arm chains of the obtained H-type polymers in order to overcome the existing methods for preparing H-type polymers. The method of object and the H type polymer prepared by this method

Method used

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Examples

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preparation example Construction

[0012] The method for preparing H-type polymer provided by the invention comprises the following steps:

[0013] (1) In the presence of a dianion initiator and a solvent, the first monomer is subjected to a two-way anionic polymerization reaction, and then an epoxy compound is used to carry out a capping reaction, and then a dihaloacyl halide is added to carry out an acylation reaction to obtain a prepolymerized thing;

[0014] (2) In the presence of a catalyst and a complexing agent, the prepolymer initiates a living free radical polymerization reaction of the second monomer.

[0015] The present invention is not particularly limited to the kind of described dianion initiator, can be the initiator of various existing bidirectional anionic polymerization that can initiate, and its example includes but not limited to: Alkali metal-naphthalene initiator, organic dilithium At least one of initiators and the like. Wherein, the alkali metal-naphthalene initiator may be at least o...

Embodiment 1

[0034] This example is used to illustrate the H-type polymer provided by the present invention and its preparation method.

[0035] Under a nitrogen atmosphere and anhydrous conditions, 1200g of benzene, 1200g of tetrahydrofuran and 120.0g (1.152mol) of styrene were added to the reactor, and then 0.6mmol of naphthalene lithium was added to initiate polymerization. After polymerization at 20°C for 2 hours, 0.1322g ( 3mmol) ethylene oxide and reacted at 20°C for 1h, then added 1.0107g (3.6mmol) 2,2-dibromoacetyl bromide and reacted at 20°C for 6h, followed by precipitation, filtration and drying to obtain 2 , 2-dibromoacetoxy terminated prepolymer, its number average molecular weight Mn=213893 and molecular weight distribution MWD=1.13 were measured by GPC.

[0036] 10.0g of the above-mentioned prepolymer was added to 500g of tetrahydrofuran, and 0.0537g of bromine was added in the ratio of bromine atom in the prepolymer: cuprous bromide: 2,2'-bipyridine molar ratio of 1:2:4 Cu...

Embodiment 2

[0039] This example is used to illustrate the H-type polymer provided by the present invention and its preparation method.

[0040] Under nitrogen atmosphere and anhydrous conditions, add 2400g toluene and 240.0g (2.305mol) styrene into the reactor, then add 2.3mmol sodium naphthalene to initiate polymerization, after polymerization at 30°C for 1h, add 0.2643g (6mmol) cyclo Oxyethane and reacted at 30°C for 0.5h, then added 2.5828g (9.2mmol) 2,2-dibromoacetyl bromide and reacted at 40°C for 1h, followed by precipitation, filtration and drying to obtain 2,2 -The prepolymer at the end of dibromoacetoxy group, the number average molecular weight Mn=107485 and the molecular weight distribution MWD=1.09 as measured by GPC.

[0041] 5.0g of the above-mentioned prepolymer was added to 500g of tetrahydrofuran, and 0.0801g of bromine was added in the ratio of bromine atom in the prepolymer: cuprous bromide: 1,10-phenanthroline molar ratio of 1:3:6 Cuprous chloride and 0.2012g of 1,10-...

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Abstract

The invention relates to the field of polymers and discloses an H-shaped polymer and a preparation method thereof. The method for preparing the H-shaped polymer comprises the following steps: (1) a first monomer is subjected to bidirectional anionic polymerization in the presence of a double anion initiator and a solvent, an end-capping reaction is performed with an epoxy compound, dihalo acyl halide is added for an acylation reaction, and a prepolymer is obtained; (2) in the presence of a catalyst and a complexing agent, the prepolymer is used for initiating an active free radical polymerization reaction of a second monomer. The H-shaped polymer with controllable molecular structure and controllable molecular weight can be prepared through conversion from bidirectional anionic polymerization to the active free radical polymerization reaction.

Description

technical field [0001] The invention relates to the field of polymers, in particular to a method for preparing H-type polymers and H-type polymers prepared by the method. Background technique [0002] The H-type structure has an important influence on the processing and rheological properties of polymers. H-type polymers have better strain hardening properties in biaxial stretching, better processability in film blow molding, and they can be used as important viscosity modifiers. At present, the method for preparing H-type polymers is mainly to utilize anionic polymerization, wherein the most commonly used method is to use a double anionic initiator to prepare a long chain with active points at both ends as a bridge, and then react with an excessive amount of silicon tetrachloride (SiCl 4 ) or methyl silicon trichloride (MeSiCl 3 ) react to form a long chain with functional groups at both ends, and then add a chain with an active point and SiCl on the bridge chain 3 -(or ...

Claims

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Application Information

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IPC IPC(8): C08F293/00C08F212/08C08F112/08
CPCC08F112/08C08F212/08C08F293/00
Inventor 王雷雷解希铭姜科李绍宁郑方远
Owner CHINA PETROLEUM & CHEM CORP
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