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A kind of bisphosphonate 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: 2018-03-30
NINGBO UNIV
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  • Abstract
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  • Claims
  • Application Information

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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 work in the organic phase However, the transition from the oil phase to the water phase cannot be achieved. The structural variability of the synthesized block polymers is not very strong, and the practical application value is limited. So far, it has not been able to be widely promoted.

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  • A kind of bisphosphonate interface initiator and preparation method thereof
  • A kind of bisphosphonate interface initiator and preparation method thereof
  • A kind of bisphosphonate 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 bisphosphonate interface initiator and a preparation method thereof. Synthesize a tertiary amine compound containing bisphosphonate anion and didodecanyl to make it exhibit a stronger emulsification function than ordinary surfactants, and at the same time, the tertiary amine can undergo redox reaction with potassium persulfate at room temperature, Cationic free radicals are first formed on nitrogen atoms, and then converted into carbon free radicals at adjacent positions. The generation of free radicals can be repeated many times, flexibly controlled, and multi-phase series polymerization is realized, which is initiated sequentially on the water / oil interface. Styrene and methyl methacrylate and styrene and hydroxyethyl acrylate to obtain multi-block copolymers. Experiments have proved that the feed ratio of monomers is very consistent with the composition ratio of copolymers, indicating that the initiator has a higher initiation efficiency. The polymerization reaction conditions of this mode are mild and controllable, the energy consumption is low, no other organic solvents and emulsifiers are used, and the product is pure, which fully meets the requirements of green chemistry.

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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Patent Type & Authority Patents(China)
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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