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Method for preparing degradable multiblock polymer

A polymer and multi-block technology, which is applied in the field of preparation of degradable multi-block polymers, can solve the problems that the number of blocks cannot be very high, and it is difficult to obtain polymers with high block numbers.

Inactive Publication Date: 2014-04-16
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

On the other hand, due to the block-by-block synthesis strategy, the number of blocks synthesized by this method cannot be very high
The number of blocks synthesized by the second method depends on the degree of reaction of the end group. When the degree of reaction of the end group is not high, it is difficult to obtain a polymer with a high number of blocks

Method used

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  • Method for preparing degradable multiblock polymer
  • Method for preparing degradable multiblock polymer
  • Method for preparing degradable multiblock polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1 uses 2-methyl-2-nitrosopropane (MNP) reaction to synthesize two-block polystyrene

[0019] Synthesis of α-brominated polystyrene (PS-Br) by atom transfer radical polymerization (ATRP) method (Journal of Polymer Science: Part A: Polymer Chemistry, 2000, 38, 2274-2283): 19.5 mg of bromide Copper (1.36×10 -4 mol) into the polymerization tube, nitrogen replacement five times. Add 186 μL of α-bromoethylbenzene (1.36×10 -3 mol), 28.4 μL N, N, N’, N”, N”-pentamethyldiethyltriamine (PMDETA) (1.36×10 -4 mol) and 3mL (2.73×10 -2 mol) styrene, reacted at 100°C for 6 hours. Gained polymer is tested through gel permeation chromatography (GPC): number average molecular weight (M n )=1110 g / mol, molecular weight distribution index (PDI)=1.10.

[0020] Diblock polymer synthesis: 12.8mg copper powder (particle size=625 mesh, 2×10 -4 mol), 112mgα-brominated polystyrene PS-Br (1×10 -4 mol) into the ampoule tube, N 2 Replaced five times. Add 1 mL of degassed solution...

Embodiment 2

[0021] Embodiment 2 uses 2-methyl-2-nitrosopropane (MNP) to synthesize two-block polyacrylate tert-butyl ester

[0022] Synthesis of α-brominated tert-butyl polyacrylate PtBA-Br by ATRP: 2-ethyl bromopropionate (2-EBP) was used as the initiator. [tBA] 0 : [2-EBP] 0 : [CuBr] 0 : [PMDETA] 0 =200:1:1:1, 25% acetone solution, react at 60°C for 3 hours. Gained polymer is tested through gel permeation chromatography (GPC): M n = 5200 g / mol, PDI = 1.18.

[0023] Diblock polymer synthesis: 12.8mg copper powder (particle size=100 mesh, 2×10 -4 mol), 520mgα-brominated polymethylacrylate PtBA-Br (1×10 -4 mol) into the ampoule tube, N 2 Replaced five times. Add 1mL degassed degassed solution containing 41μL PMDETA (2×10 -4 mol), 4.4mg MNP (5×10 -5 mol) THF solution. React at 100°C for 0.1 hour. The polymer was dissolved in tetrahydrofuran, passed through a column of neutral alumina to remove copper, concentrated, precipitated with methanol, and dried under vacuum at 50°C over...

Embodiment 3-7

[0024] Embodiment 3-7 uses 2-methyl-2-nitrosopropane (MNP) reaction to synthesize multi-block polystyrene

[0025] Synthesis of α,ω-brominated polystyrene Br-PS-Br by ATRP: 2,5-dibromodiethyl adipate (DEDBA) was used as the initiator. [St] 0 : [DEDBA] 0 : [CuBr] 0 : [PMDETA] 0 =20:1:0.2:0.2, react at 100°C for 80 minutes. Gained polymer is tested through gel permeation chromatography (GPC): M n = 1260 g / mol, PDI = 1.10.

[0026] Multi-block polystyrene synthesis: 14mg copper powder (particle size=625 mesh, 2.2×10 -4 mol), 130mgα, ω-brominated polystyrene Br-PS-Br (1×10 -4 mol) into the ampoule tube, N 2 Replaced five times. Add 1mL degassed degassed solution containing 41μL PMDETA (2×10 -4 mol), 8.7mg MNP (1×10 -4 mol) THF solution. The reaction was carried out at room temperature for different times, and the reaction was terminated. The polymer was dissolved in acetone, passed through an alumina column to remove copper, concentrated, fractionated and purified by ...

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Abstract

The invention discloses a method for preparing a degradable multiblock polymer, which comprises the following steps of: adding 1mol of polymer with the terminal functional group of halogen, 0.5-5mol of radical capture agent, 2-10mol of metal copper or copper salt and 2-10mol of polyamine into a reactor under the condition of the existence of a solvent; and after stirring and deoxidizing, reacting at 10-100 DEG C for 0.1-24 hours to obtain the degradable multiblock polymer. The invention has the advantages of simple synthesizing method and mild reaction condition and can be used for synthesizing multiblock polymers with different monomer types and block number, and the block number can exceed 30 blocks. The degradable multiblock polymer can be also prepared by reacting the polymer with a main chain of different monomers and the terminal functional group of halogen with the radical capture agent. When the multiblock polymer is heated to certain temperature, the multiblock polymer can be degraded to obtain a monodispersed low-molecular weight oligomer.

Description

technical field [0001] The invention relates to a preparation method of a polymer, in particular to a preparation method of a degradable multi-block polymer. Background technique [0002] Multi-block polymers are formed by linking different polymer segments, and can exhibit different properties depending on the linking polymers. For example, linking soft segments with hard segments, linking light water with hydrophobic segments, or linking crystalline and amorphous segments, the resulting multi-block copolymer materials can exhibit some unconventional properties or morphologies. It can be used in the development of new surfactants, thermoplastic elastomers and compatibilizers for polymer blends. [0003] There are two main methods for the synthesis of traditional multi-block copolymers. The first is to continuously add new and different monomers to the active polymerization system to prepare polymers segment by segment, which can be called segment-by- segment method. The ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F293/00
Inventor 张成裕王齐
Owner ZHEJIANG UNIV