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Polymer of terminal dihydroxy, and prepartion method

A technology of end-dihydroxyl-functionalized polymers, applied in the field of end-group functionalized polymers, can solve the problems of incomplete functionalization and conversion of polymer end-groups, and achieve the effects of controllable molecular weight, clear structure and high initiation efficiency

Inactive Publication Date: 2008-12-17
山东科尔本高分子新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above method still has the disadvantage of incomplete functional conversion of polymer end groups.

Method used

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  • Polymer of terminal dihydroxy, and prepartion method
  • Polymer of terminal dihydroxy, and prepartion method
  • Polymer of terminal dihydroxy, and prepartion method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Example 1 Preparation of tert-butyldimethylsiloxypropyllithium:

[0041]In a 250ml three-necked flask, 38g (0.4mol) of 3-chloro-1-propanol, 61g (0.4mol) of tert-butyldimethylsilyl chloride, and 80ml of DMF were sequentially added. Then a DMF (30ml) solution containing 30g (0.44mol) of imidazole was added dropwise to the reaction system within 0.5h at 0°C, under N 2 Stir overnight at room temperature under air protection. Add 350ml n-hexane, then 300ml 5% NaHCO 3 The aqueous solution was washed three times, and the n-hexane layer was separated. with anhydrous MgSO 4 After drying, the solvent was evaporated by rotary evaporation, and a colorless liquid was obtained by column separation with a yield of 94%.

[0042] Under Ar atmosphere, add 8g (1.01mol) lithium and 50ml anhydrous cyclohexane to a 250ml three-necked flask equipped with a condenser, a constant pressure dropping funnel, and magnetic stirring. mol) tert-butyl-(3-chloropropoxy)dimethylsilane in cyclohexane...

Embodiment 2

[0043] Example 2 Preparation of tert-butyldimethylsiloxane-2,2-dimethylpropyl lithium

[0044] In a 250ml three-necked flask, 49.0g (0.4mol) of 3-chloro-2,2-dimethyl-1-propanol, 61g (0.4mol) of tert-butyldimethylsilyl chloride, and 100ml of DMF were sequentially added. Then a DMF (30ml) solution containing 30g (0.44mol) of imidazole was added dropwise to the reaction system within 0.5h at 0°C, under N 2 Stir overnight at room temperature under air protection. Add 350ml of n-hexane, then use 300ml of 5% NaHCO 3 The aqueous solution was washed three times, and the n-hexane layer was separated. with anhydrous MgSO 4 After drying, the solvent was evaporated by rotary evaporation, and a colorless liquid was obtained by column separation with a yield of 93%.

[0045] Under Ar atmosphere, add 8g (1.01mol) of lithium and 50ml of anhydrous cyclohexane into a 250ml three-necked flask equipped with a condenser, a constant pressure dropping funnel, and magnetic stirring. mol) tert-bu...

Embodiment 3 3

[0046] The preparation of embodiment 3 trimethylsiloxyhexyllithium:

[0047] In a 250ml three-necked flask, 48.2g (0.4mol) of 6-chloro-1-hexanol, 43.4g (0.4mol) of trimethylchlorosilane, and 80ml of DMF were sequentially added. Then a DMF (30ml) solution containing 30g (0.44mol) of imidazole was added dropwise to the reaction system within 0.5h at 0°C, under N 2 Stir overnight at room temperature under air protection. Add 350ml n-hexane, then 300ml 5% NaHCO 3 The aqueous solution was washed three times, and the n-hexane layer was separated. with anhydrous MgSO 4 After drying, the solvent was evaporated by rotary evaporation, and a colorless liquid was obtained by separation through a chromatographic column with a yield of 92%.

[0048] Under Ar atmosphere, add 8g (1.01mol) lithium and 50ml anhydrous cyclohexane to a 250ml three-necked flask equipped with a condenser, a constant pressure dropping funnel, and magnetic stirring. mol) cyclohexane (50ml) solution of trimethyl(...

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Abstract

This invention relates to a method for preparing dihydroxyl-terminated telechelic polymer. The method uses an initiator that can be easily hydrolyzed and is protected by silicane protective groups. The initiator has such advantages as high stability and high initiation efficiency, and has wide industrial applications. The initiator can initiate anion polymerization of 1,3-dialkene, styrene and acrylate monomers to form dihydroxyl-terminated homopolymers and copolymers. The synthesized dihydroxyl-terminated polymers have such advantages as clear structure, controllable molecular weight, controllable chain microstructure and high functional yield.

Description

technical field [0001] The invention belongs to the field of end-group functionalized polymers, and relates to a preparation method of end-dihydroxyl polymers, that is, anionic polymerization is used to prepare end-dihydroxyl oligomers by using organolithium initiators containing organosilicon protection groups. Background technique [0002] Terminal-functionalized polymers have special application value due to their special molecular structure, such as hydroxyl-terminated polybutadiene, which has been used as a binder for solid rocket propellants, in coatings, sealants and adhesives There are also applications. In addition, it can also be copolymerized with suitable materials to form polyethers, polycarbonates and polyamides. It has very important uses in aerospace, military industry and civil use. [0003] The synthesis of terminal dihydroxy polymers (such as polybutadiene) generally adopts the free radical polymerization method in industry, and its advantages are simple...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F36/02C08F12/08C08F20/26C08F4/48C08F8/00
Inventor 鲁在君李美顺孙强强
Owner 山东科尔本高分子新材料有限公司