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Method for preparing copolymer with multielement alternating structure

A technology of alternating structure and copolymer, which is applied in the field of preparation of copolymers, can solve problems such as side reactions and low molecular weight of polymers, and achieve a wide range of effects

Inactive Publication Date: 2011-04-13
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this reaction has certain limitations, there is a certain proportion of side reactions, and the molecular weight of the obtained polymer is also low

Method used

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  • Method for preparing copolymer with multielement alternating structure
  • Method for preparing copolymer with multielement alternating structure
  • Method for preparing copolymer with multielement alternating structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 12

[0022] Embodiment 12, 5-dibromodiethyl adipate (DEDBA) reacts with 2-methyl-2-nitrosopropane (MNP)

[0023] Add 70.4mg Cu powder (1.1mmol), 180mg DEDBA (0.5mmol), 43.5mg MNP (0.5mmol) into the ampoule tube, and replace with nitrogen three times. Add 208 μL (1 mmol) of PMDETA that has been deoxygenated, and THF 1 mL. At 25°C, react for 30 minutes, and quench with liquid nitrogen to terminate the reaction. The polymer was dissolved in acetone, passed through a column of neutral alumina to remove copper, concentrated, and dried under vacuum at 50°C for 24 hours. Gained polymer is tested through gel permeation chromatography (GPC): number average molecular weight (M n ) = 8360 g / mol, molecular weight distribution index (PDI) = 2.35.

Embodiment 22

[0024] Example 22, 7-dibromosuberate dimethyl (DMDBO) reacts with 2-methyl-2-nitrosopropane (MNP)

[0025] Synthesis of dimethyl 2,7-dibromosuberate (DMDBO): Add 5.23g (0.03mol) of suberic acid and 5.4mL (0.075mol) of thionyl chloride into a 25mL Schlenk bottle and heat to 80°C , reacted for 1.5 hours. The heating was stopped, and the remaining thionyl chloride was removed from the Schlenk bottle. The Schlenk bottle was heated to 85°C, and 3.9mL (0.076mmol) of liquid bromine (Br 2 ) slowly added to the Schlenk bottle several times (0.5 mL each time), and the addition was completed within 6 hours. Stirring was continued at 85°C for 3 hours. The hot reaction solution was added dropwise into 50 mL of ice-cooled anhydrous methanol solution, raised to room temperature, and stirred overnight. The methanol solution was poured into deionized water at 0 °C to obtain a yellow turbid liquid. With 5×30mL CH 2 Cl 2 Extract and combine the organic layers. The organic layer was washe...

Embodiment 3-8

[0027] Example 3-8 Reaction of 2,13-dibromotetradecanedioic acid dimethyl ester (DMDBT) with 2-methyl-2-nitrosopropane (MNP)

[0028] Synthesis of 2,13-dibromotetradecanedioic acid dimethyl ester (DMDBT): 5.16g (0.02mol) tetradecanedioic acid, 4.3mL (0.06mol) thionyl chloride were added to a 25mL Schlenk bottle, Heated to 80°C and reacted for 1.5 hours. The heating was stopped, and the remaining thionyl chloride was removed from the Schlenk bottle. The Schlenk bottle was heated to 85°C, and 2.6mL (0.05mmol) of Br 2 Slowly add to the Schlenk bottle several times (0.5 mL each time) and complete the addition within 4 hours. Stirring was continued at 85°C for 3 hours. The hot reaction solution was added dropwise into 40 mL of anhydrous methanol solution cooled in an ice bath, raised to room temperature, and stirred overnight. The methanol solution was poured into 80 mL of deionized water at 0 °C to obtain a yellow turbid liquid. With 5×30mL CH 2 Cl 2 Extract and combine the...

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Abstract

The invention discloses a method for preparing a copolymer with a multielement alternating structure. The method comprises the following steps of: in the presence of a solvent, adding 1mol of nitroso compound, 0.5 to 5mol of dibromo compound, 1 to 10mol of metallic copper or copper salt and 1 to 10mol of polyamine to a reactor and stirring, and reacting for 0.1 to 24 hours at the temperature of 10 to 100 DEG C after deoxidized to obtain the copolymer with the multielement alternating structure. The invention has simple synthetic method and mild reaction condition and can utilize the dibromo compound with different structures to be reacted with the nitroso compound to obtain the copolymer with the multielement alternating structure. The invention overcomes defects of the traditional methods, synthesizes the high molecular weight (Mn>50,000g / mol) copolymer with the multielement alternating structure, and expands the new method for synthetizing high molecules.

Description

technical field [0001] The invention relates to a preparation method of a polymer, in particular to a preparation method of a copolymer with multiple alternating structures. Background technique [0002] Synthesizing polymers with multiple alternating structures is a goal and challenge in the field of polymer synthesis. Although polymers containing multiple monomer units can be obtained by traditional copolymerization, it is difficult to precisely control the sequence structure of comonomers. Only some special monomers can be copolymerized to obtain strictly binary alternating structure copolymers, such as styrene and maleic anhydride. In recent years, articles on the control of polymer sequence structures have been reported from time to time, but the existing methods are still unable to achieve complete controllable polymerization of the secondary structure of polymers. Nevertheless, there are quite a few examples that show us the possibility of achieving this goal (Polym...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/00
Inventor 张成裕王齐
Owner ZHEJIANG UNIV
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