A kind of vinyl polar monomer implements the method for anionic addition polymerization

A technology of anionic polymerization and polar monomers, which is applied in the field of anionic addition polymerization of vinyl polar monomers, can solve the problem that the stability needs to be further improved, and can enrich the varieties of high-performance polymers and suppress side reactions. Effect

Active Publication Date: 2017-03-15
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this technology needs to be polymerized at a relatively low temperature of around 0°C, and the stability still needs to be further improved

Method used

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  • A kind of vinyl polar monomer implements the method for anionic addition polymerization
  • A kind of vinyl polar monomer implements the method for anionic addition polymerization
  • A kind of vinyl polar monomer implements the method for anionic addition polymerization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Example 1: Preparation of polymethyl methacrylate (PMMA)

[0034] At 20°C, under the premise that the water in all reagents is less than 10ppm, add 48ml of THF to the reaction kettle, add 0.001mol of 0.1M n-butyllithium (n-BuLi), and then add 0.198g of DPE to react for 10min. Then add 2.24g (0.02mol) potassium tert-butoxide (t-BuOK), react for 10min, then add 10g MMA monomer and stir evenly, and the designed molecular weight is 10,000. After 20 min of reaction, the polymer active species were terminated with 1 ml of methanol. The conversion rate is shown in Table 1, the molecular weight of the product and its distribution are determined by GPC, and the results are shown in Table 1.

Embodiment 2

[0041] Example 2: Polymerization of polystyrene-polybutadiene-polymethylmethacrylate triblock polymerization (PS-b-PB-b-PMMA)

[0042] At 50°C, under the premise that the water in all reagents is less than 10ppm, add 48ml toluene to the reaction kettle under the protection of 0.4MPa high-purity argon, add 0.1M tert-butyllithium (t-BuLi) 0.00025mol, styrene (St) 1.25g (design molecular weight 5000), after 10min of polymerization, add 7.5g of butadiene (Bd) (design molecular weight 30000), and polymerize for 20min. The system was cooled to 10° C., 0.66 g (0.005 mol) of potassium phenate was added, stirred uniformly, and reacted for 10 min. Add MMA 2.5g, about 2.65ml, the designed molecular weight is 10000. The reaction was carried out for 20 minutes. After the reaction was completed, the polymer active species was terminated with 1 ml of methanol. The conversion rate is shown in Table 2, the molecular weight of the product and its distribution are determined by GPC, and the r...

Embodiment 3

[0048] Example 3: Polymerization of polymethyl methacrylate and tert-butyl methacrylate diblock copolymer [P(t-BMA)-b-PMMA]

[0049] Under the premise that the water in all reagents is less than 6ppm at 60°C, add 60ml of THF to the reaction kettle, add 0.1M n-BuLi 0.0005mol, DPE 0.1g (0.00055mol), stir evenly, and react for 10min. Add 1.82 g (0.01 mol) of potassium naphthol, stir evenly, and react for 10 min. 7.5 g of tert-butyl methacrylate (t-BMA) was added, and the designed molecular weight was 15,000. After 10min of polymerization, 4g of MMA was added, and the designed molecular weight was 8000, and the reaction was carried out for 20min. After the reaction, the active species of the polymer were terminated with 1 ml of methanol. The conversion rate is shown in Table 3, the molecular weight of the product and its distribution are determined by GPC, and the results are shown in Table 3.

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Abstract

The invention relates to a method for carrying out anionic addition polymerization on a polar vinyl monomer. The method comprises the following steps: firstly, reducing water in all the adopted reagents to be less than 10ppm, then adding a reactive species, diphenylethylene or triphenyl diethylene, excess K-O-Ar, at least one polar vinyl monomer and / or at least one non-polar vinyl monomer into an organic solvent, and carrying out reaction between the room temperature and the temperature of 60 DEG C to realize anionic addition polymerization. The Li countra-ions in the reactive species can be converted into the K countra-ions due to the adoption of excess K-O-Ar, the side reaction during anionic polymerization of the polar vinyl monomer can be inhibited effectively due to the adoption of the inactive Li-O-Ar, and the anionic polymerization can be carried out between the room temperature and the temperature of 60 DEG C. The method provided by the invention is used for carrying out anionic polymerization on widely used monomers on a feasible industrial level to generate abundant segmented, telechelic, branched and star-shaped high-performance polymers in complex structures.

Description

technical field [0001] The present invention relates to polymer material polymerization technology, in particular to a method for carrying out anionic addition polymerization of vinyl polar monomers. Background technique [0002] Anionic polymerization has been widely used in the field of polymer synthesis, which is characterized by rapid initiation, rapid growth, almost no termination, controllable molecular weight of the product, narrow molecular weight distribution, and clear structure. Under appropriate conditions (the system is very pure), anionic polymerization can not occur chain termination or chain transfer reaction, 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 be Functionalized telechelic polymers or block copolymers of various structures are obtained. However, because the anionic polymerization reaction is very fast, a large amoun...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F120/14C08F297/04C08F297/02C08F4/48
Inventor 管涌郑安呐束明泽危大福李铮占鹏飞邹斌
Owner EAST CHINA UNIV OF SCI & TECH
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