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Method for controlling anionic polymerization reaction

An anionic polymerization and reaction technology, applied in the field of initiator associations, can solve problems such as by-products and inaccurate metering, adverse effects of direct functionalization steps of products, etc., and achieve the effect of improving difficulty

Inactive Publication Date: 2011-06-08
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Furthermore, such complexes also have strong nucleophilicity, which has adverse effects on the subsequent direct functionalization steps of the product.
For example, the synthesis process of hydroxyl-terminated polybutadiene is that ethylene oxide is directly added in the final stage of the anionic polymerization of butadiene, and then terminated with methanol to obtain the target product; but if there are organic magnesium or organic aluminum remaining in the system compound, it will undergo a ring-opening reaction with the added ethylene oxide, resulting in by-products and inaccurate metering
Therefore, both in theory and in practical application, this kind of complexes has big problems.

Method used

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  • Method for controlling anionic polymerization reaction
  • Method for controlling anionic polymerization reaction
  • Method for controlling anionic polymerization reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Embodiment 1: the preparation of polystyrene (PS)

[0034] At room temperature, add 48ml of cyclohexane to the reaction kettle, add lithium phenate (initiator association) and sodium naphthalene (initiator) in equimolar ratio, stir evenly, add 12ml of styrene monomer, the design molecular weight is 10,000. Gradually raise the temperature to 50°C and react for 2 hours. After the reaction, the polymer active species was terminated with 1 ml of methanol. The conversion rate is shown in Table 1, and the molecular weight and distribution of the product are determined by GPC, and the results are shown in Table 1.

Embodiment 2

[0040] Embodiment 2: Polymerization of polymethyl methacrylate (PMMA)

[0041] At 0°C, add 48ml of toluene to the reaction kettle, add lithium naphthate (initiator association) and diphenylhexyllithium (initiator) in equimolar ratio, through n-butyllithium and 1,1-diphenylethylene equimolar reaction), stir evenly, add 5ml methyl methacrylate (MMA), the design molecular weight is 2500. Gradually raise the temperature to 20°C and react for 20 minutes. After the reaction, the polymer active species was terminated with 1 ml of methanol. The conversion rate is shown in Table 2, and the molecular weight and distribution of the product are determined by GPC, and the results are shown in Table 2.

Embodiment 3

[0047] Embodiment 3: Polymerization of polymethyl methacrylate and tert-butyl methacrylate diblock copolymer (PMMA-PtBMA)

[0048] At 0°C, add 60ml of toluene to the reaction kettle, add lithium hydroquinone (initiator association) and diphenylhexyllithium (initiator) in equimolar ratio, through n-butyllithium and 1,1-diphenyl base ethylene equimolar reaction), stirred evenly, added 5ml methyl methacrylate (MMA), the design molecular weight was 2500. Gradually raise the temperature to 20°C and react for 20 minutes. After the reaction, tert-butyl methacrylate (tBMA) (7.66ml, design molecular weight: 3550) was added in equimolarity with MMA, reacted at the same temperature for 30min, and then terminated the polymer active species with 1ml methanol. The conversion rate is shown in Table 3, and the molecular weight and distribution of the product are determined by GPC, and the results are shown in Table 3.

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Abstract

The invention relates to a method for controlling anion polymerization, wherein initiator association complexes are directly added into monomers or an initiator by means of a solution simultaneously or respectively at different moment or in different stages for anion polymerization; metallic atoms of the initiator association complexes are associated with cations of the initiator; limitation of the polymerization speed is realized by utilization of oxyl with large volume or large steric hindrance to limit a monomer addition channel, and side reaction is inhibited; and the polymerization temperature is controlled and adjusted, and anion polymerization can be performed when the polymerization temperature is raised to the room temperature or a higher temperature, wherein the mol ratio of theinitiator association complexes to the initiator is between 0.01 to 1 and 20 to 1. Compared with the prior art, the method can control and adjust the homopolymerization speed, the copolyreaction speed, side reaction and the polymerization temperature of various anion polymeric monomers, and is easy to realize industrial production.

Description

technical field [0001] The invention relates to the technical field of polymer material polymerization, in particular to a new method for controlling and adjusting anionic polymerization speed, side reactions and polymerization temperature and an initiator association used in the method implementation process. Background technique [0002] Anionic polymerization has been widely used in the field of polymer synthesis, which is characterized by fast initiation, fast growth, almost no termination, controllable molecular weight of the product, narrow molecular weight distribution, and clear structure. Anionic polymerization under proper conditions (the system is very pure), no chain termination or chain transfer reaction can occur, and the active chain can still maintain polymerization activity until the monomer is completely exhausted; if an appropriate end-capping agent or a second monomer is added, it can Functionalized telechelic polymers or block copolymers of various struc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F2/00C08F2/06C08F2/38C08F4/48C08F297/02
Inventor 郑安呐张健管涌胡福增危大福王书忠
Owner EAST CHINA UNIV OF SCI & TECH