Preparation method of ultra-high graft density polymer molecular brush

A graft density and polymer technology is applied in the field of preparation of ultra-high graft density polymer molecular brushes, and can solve the problems of difficult preparation of ultra-high graft density polymer molecular brushes.

Active Publication Date: 2019-03-01
浙江理工大学上虞工业技术研究院有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the steric hindrance and volume repulsion between molecular brush chains...

Method used

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  • Preparation method of ultra-high graft density polymer molecular brush
  • Preparation method of ultra-high graft density polymer molecular brush
  • Preparation method of ultra-high graft density polymer molecular brush

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preparation example Construction

[0033] The invention provides a kind of preparation method of ultra-high grafting density polymer molecular brush, comprises the following steps:

[0034] (1) Immerse the monocrystalline silicon wafer in the mixed solution of concentrated sulfuric acid and aqueous hydrogen peroxide solution, heat treatment, and then wash and dry the heated monocrystalline silicon wafer sequentially to obtain SiO 2 / Si substrate;

[0035] (2) the SiO that described step (1) obtains 2 / The Si substrate is immersed in the initiator solution and subjected to static treatment to obtain the initiator-functionalized SiO 2 / Si substrate; The initiator is 22-(trichlorosilyl) docosyl-2-bromo-2-phenylacetate;

[0036] (3) under nitrogen protection, the initiator functionalized SiO that described step (2) obtains 2 / Si substrate, cuprous bromide, styrene, pentamethyldiethyltriamine and toluene are mixed and then heat-treated to obtain ultra-high graft density polymer molecular brushes.

[0037] In th...

Embodiment 1

[0102] Synthesis of 21-dodecen-1-ol: Add magnesium chips (1.68g, 70mM) and freshly distilled tetrahydrofuran (2mL) to a 250mL three-necked flask under nitrogen atmosphere, add a few drops of 1,2-dibromo Ethane activates magnesium chips. Then, a solution of 1-bromo-undecene (11.65 g, 0.05 mol) in freshly distilled tetrahydrofuran (50 mL) was added dropwise, and moderate reflux was controlled after a few minutes, and the temperature in the three-necked flask did not exceed 55°C. After the dropwise addition, the reaction mixture was heated at 50°C for 2 hours, then cooled to -78°C, and maintained at this temperature for 20 minutes, purified CuI (0.38g, 2mM) was added under nitrogen flow, and the mixture was heated at -78°C Leave on for 10 minutes. Then, slowly warm up to 0°C until dark purple appears, immediately cool to -78°C and add protected alcohol solution (10.28g, 0.04mol, in 50mL THF), (protected alcohol solution consists of 0.04mol 11-bromo-1 - undecanol, 0.04mol methyl...

Embodiment 2

[0112] The test was carried out according to the method of Example 1, with the difference that in the preparation process of the polymer molecular brush, the heating time in the oil bath was adjusted to 130 minutes to obtain a polystyrene molecular brush.

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Abstract

The invention relates to the field of polymer synthesis. The invention provides a preparation method of an ultra-high graft density polymer molecular brush. The method comprises the following steps: firstly, preparing a SiO2/Si substrate by using a single-crystal silicon wafer, and then self-assembling an initiator monomolecular layer on the surface of the SiO2/Si substrate, wherein an initiator is 22-(trichlorosilyl)docosa-2-bromo-2-phenylacetate; finally, under nitrogen protection, enabling the product to react with cuprous bromide, styrene, pentamethyl diethyl triamine and toluene to prepare the ultra-high graft density polymer molecular brush. The results of the embodiments show that the thickness of the polymer molecular brush is 55-65 nm, and the graft density of the polymer molecular brush is 1.21-1.23 chains/nm<2>.

Description

technical field [0001] The invention relates to the field of macromolecule synthesis, in particular to a preparation method of an ultra-high graft density polymer molecular brush. Background technique [0002] Polymer molecular brush is a special polymer assembly system. One end of its molecular chain is fixed on the solid surface through a covalent bond, which can effectively adjust the physical and chemical properties of the solid surface. It is used in colloidal stabilizers, biological materials, marine antifouling, Lubrication and microelectronics industry and other fields have a wide range of applications. For example, in the field of biomaterials, by preparing hydrophilic polymer molecular brushes on the solid surface, the non-specific interaction between the solid surface and proteins can be weakened, such as the deposition of biological cells, bacteria, etc. on the surface or interface. [0003] The grafting density of polymer molecular brushes determines the confor...

Claims

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Application Information

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IPC IPC(8): C08F292/00C08F212/08
CPCC08F292/00C08F212/08
Inventor 左彪李成王新平
Owner 浙江理工大学上虞工业技术研究院有限公司
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