Diphosphonate interface initiator and preparation method thereof

A bisphosphonate and initiator technology, applied in the field of polymer material synthesis, can solve the problems that the structure of block polymers is not very variable, the practical application value is limited, and cannot be widely promoted, and the polymerization reaction conditions are mild and acceptable. control, fast polymerization reaction and high conversion rate

Active Publication Date: 2016-08-24
NINGBO UNIV
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Problems solved by technology

In recent years, living free radical polymerization technology has been greatly developed, and the way of free radical initiation has been improved, thus making the synthesis of block copolymers easier and more convenient, but these living free radical polymerizations generally only wo

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  • Diphosphonate interface initiator and preparation method thereof
  • Diphosphonate interface initiator and preparation method thereof
  • Diphosphonate interface initiator and preparation method thereof

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Embodiment Construction

[0019] Below in conjunction with embodiment the present invention is described in further detail.

[0020] Preparation of bisphosphonate interfacial initiator:

[0021] 1. Mix and dissolve dodecylamine and epichlorohydrin in absolute ethanol as far as possible according to the molar ratio of 2:1. The weight ratio of dodecylamine to ethanol is controlled in the range of 1:4.5 to 1:5. Control the reaction temperature in the range of 50-60°C, and the reaction time is 3-4 hours. After the reaction is completed, cool to room temperature, add solid NaOH, and stir continuously to dissolve NaOH;

[0022] 2. Add epichlorohydrin to the above reaction liquid again, and control the molar ratio of epichlorohydrin to dodecylamine at 1:1 as much as possible, and control the reaction temperature in the range of 25-30°C under stirring, and react for 10-12 After one hour, cool to room temperature and add solid NaOH. The mole number of NaOH should be the same as the mole number of epichlorohydr...

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Abstract

The invention relates to a diphosphonate interface initiator and a preparation method thereof. A tertiary amine compound containing diphosphonic acid radical anions and didodecyl groups is firstly synthesized to enable the tertiary amine compound to show the emulsifying function which is higher than that of a common surfactant, tertiary amine can generate a redox reaction with potassium persulfate at room temperature, cation free radicals are firstly formed on nitrogen atoms and then converted into carbon free radicals at the adjacent positions, generation of the free radicals can be repeated for multiple times and flexibly controlled, multiphase concatenating polymerization is achieved, polymerization of styrene and methyl methacrylate and polymerization of styrene and hydroxyethyl acrylate are initiated on a water-oil interface in sequence, and then a segmented copolymer is obtained. Experiments prove that the feed ratio of monomers is quite consistent with the component ratio of the copolymer, that is to say, the initiation efficiency of the initiator is very high, this mode of polymerization reaction is mild and controllable in condition and low in energy consumption, no other organic solvent or emulsifier is used, the product is pure, and the requirements of green chemistry are totally met.

Description

technical field [0001] The invention relates to the technical field of polymer material synthesis, in particular to a bisphosphonate interface initiator and a chemical preparation method thereof. The novel initiator can be used for the green synthesis of polyolefin polymer materials. Background technique [0002] Polyolefin is a very important general-purpose polymer material with adjustable structure and wide application. These materials are generally obtained by homopolymerizing or copolymerizing olefin monomers through free radical initiators. According to different polymerization occasions, initiators can be divided into two categories: oil-soluble and water-soluble, corresponding to oil-soluble and water-soluble monomers respectively. polymerization. Ordinary initiators are only a class of compounds that can generate free radicals, such as oil-soluble peroxides, azo initiators, and water-soluble persulfates. The use of initiators must be matched with the specific polym...

Claims

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Application Information

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IPC IPC(8): C08F4/40C07F9/38
Inventor 孙怀艳张瑞丰李伟逊尚传洋江峰肖通虎龙能兵
Owner NINGBO UNIV
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