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Structure-controllable polymethylene macro-molecule initiating agent and preparation method and application thereof

A technology of macromolecular initiator and polymethylene, which is applied in the field of polymethylene macroinitiator, can solve the problems of group conversion and preparation of macromolecular initiator, etc.

Inactive Publication Date: 2013-10-30
SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although they and other research groups have carried out some group conversion work on this type of polymer [US5476915; Macromolecules 2000, 33, 4295], they have not used it to perform group conversion to prepare macromolecular initiators

Method used

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  • Structure-controllable polymethylene macro-molecule initiating agent and preparation method and application thereof
  • Structure-controllable polymethylene macro-molecule initiating agent and preparation method and application thereof
  • Structure-controllable polymethylene macro-molecule initiating agent and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] The preparation of the macroinitiator based on polyolefin with controllable structure of the present invention:

[0048] (1) Preparation of main chain terminal hydroxyl polyolefin

[0049] In a dry 500mL three-neck flask equipped with a reflux condenser, pass N 2 Add 3113g (0.242mol) of trimethylthionyl chloride under the state, add 7.55g (0.315mol) of NaH, add dry 250mL toluene with a syringe, reflux for 5h, filter the obtained gray suspension to obtain the toluene of ylide solution (concentration is 0.6mmol / mL).

[0050] In a dry 500mL three-necked flask equipped with a magnetic stirrer and a reflux condenser, N 2 Add 300mL (0.18mol) of the above-mentioned ylide toluene solution through a syringe under protection, stir at room temperature, and quickly add 0.60mL (0.60mmol) of BH 3 ·SMe 2 (Yi Lide / BH 3 ·SMe 2 molar ratio = 300), slowly warming up to 75°C. After reacting for 1 hour, cool down to room temperature, add 0.40 g (3.60 mmol) trimethylammonium oxide dih...

Embodiment 2～ Embodiment 12

[0054] The preparation of the controllable polymethylene macromolecular initiator of structure of the present invention:

[0055] Operation is basically the same as embodiment 1. The difference is that PM 1 -OH consumption, the type and amount of compound (I) in the esterification reaction process, the type and amount of catalyst, reaction solvent, reaction temperature, and reaction time are not completely the same as in Example 1. The structure-controllable polymethylene macroinitiator PM was obtained by the reaction 1 -(X) 2 . Wherein, X is Cl or Br, and the subscript "2" outside the brackets means two Xs.

[0056] The specific experimental conditions and polymer characterization data are shown in Table 1:

[0057] Table 1

[0058]

[0059] Note: PM 1 The amount of -OH is 0.67g (0.76mmol, 1 equiv.); the amount of solvent is 30mL; the conversion rate of the group is ~100%;

[0060] Obtain structure controllable polymethylene macromolecule initiator PM in embodiment...

Embodiment 10

[0063] The preparation of the polyolefin-based macromolecular initiator with controllable structure of the present invention:

[0064] (1) Preparation of main chain terminal hydroxyl polyolefin

[0065] Operation is basically the same as embodiment 1. The difference is that BH 3 ·SMe 2 The dosage is 0.4mL (0.4mmol) (Yet / BH 3 ·SMe 2 Molar ratio=600), the consumption of trimethylammonium oxide dihydrate is 0.27g (2.4mmol). To obtain the main chain terminal hydroxyl polyolefin PM 2 -OH(M n (GPC) = 1800 g / mol, PDI = 1.08, hydroxyl content = 0.35 mmol / g).

[0066] (2) Esterification reaction

[0067]In a dry 100mL round-bottomed flask with a condenser and a magnetic stirrer, add 3.0g (1.05mmol OH, 1 equiv.) of the product PM obtained above under nitrogen protection 2 -OH, 1.5mL (10.5mmol, 12equiv.) Catalyst triethylamine (TEA) and 120mL of toluene, stirring and dissolving at 90°C and cooling down to room temperature, then slowly dripping 5.0mL (51.8mmol, 12.2 equiv.) comp...

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Abstract

The invention discloses a structure-controllable polymethylene macro-molecule initiating agent, a preparation method and an application thereof. The structure-controllable polymethylene macro-molecule initiating agent can be regulated and controlled in number-average molecular weight within a certain range of 900-1.42*10<4> g / mol and has a narrow molecular weight distribution PDI=1.04-1.18. Various polymethylene macro-molecule initiating agents with controllable molecular weight and narrow molecular weight distribution are prepared through an esterifying reaction from main chain hydroxy-terminated polymethylene with the controllable molecular weight and the narrow molecular weight distribution, and the main chain hydroxy-terminated polymethylene is obtained through ylide living polymerization; and the polymethylene macro-molecule initiating agents are applied to the atom transfer radical polymerization of a polymerizable monomer, so that a three-arm block polymer is prepared.

Description

technical field [0001] The invention relates to a structurally controllable polymethylene macromolecular initiator, a preparation method and an application thereof, and belongs to the technical field of polyolefin functionalization. Background technique [0002] Polyolefin material is a polymer material widely used in many fields such as industry, agriculture and daily life. However, polyolefin is composed of saturated hydrocarbon molecular units, its molecular chain is non-polar, and its compatibility with other materials, especially polar materials, is very poor, so the expansion of its application range is limited to a certain extent. . For a long time, the introduction of polar functional groups or polar polymer segments into polyolefin macromolecular chains to increase the polarity of polyolefins and expand their application fields has become one of the hotspots in academia and industry. [0003] The functionalization methods of polyolefins can be roughly divided into...

Claims

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Application Information

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IPC IPC(8): C08F293/00C08F110/00C08F8/14
Inventor 马志薛扬赵巧玲黄晋
Owner SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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