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Production method of spiral bi-thienyl silicon oxide nanometer material

A technology of bithienyl silicon oxide and nanomaterials, which is applied in the field of nanomaterials to achieve the effects of cheap raw materials, convenient operation and easy availability of raw materials

Inactive Publication Date: 2012-07-04
苏州苏凯路化学科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And bithienyl silica, especially the bithienyl silica with helical structure, has not been reported yet.

Method used

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  • Production method of spiral bi-thienyl silicon oxide nanometer material
  • Production method of spiral bi-thienyl silicon oxide nanometer material
  • Production method of spiral bi-thienyl silicon oxide nanometer material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] by L Preparation of 4,4'-bithienyl silica with alanine-type cationic surfactant as template.

[0038] (1) L Synthesis of -18Ala6Et3Br

[0039] 111.6g (0.5 mol) benzyloxy protected L -Alanine (Z- L -Ala ) was dissolved in 400 mL ethyl acetate, and 113.3 g (0.55 mol) DCC was added under ice-water bath, and stirred for 1.0 h. Dissolve 134.8 g (0.5 mol) NH with ethyl acetate 2 (CH 2 ) 17 CH 3, added to the three-necked flask after cooling, and stirred for 2.0 h. Stir at room temperature for 1.5 h, in an oil bath at 45°C for 48.0 h, and at 60°C for 3.0 h. Add 10.0 mL of glacial acetic acid and continue stirring for 1.0 h. The reaction mixture was filtered while it was hot, and the filtrate was cooled in an ice-water bath. After suction filtration, the solid was collected and recrystallized with n-propanol to obtain the intermediate product Z- L -Ala-NH-C 18 h 37 .

[0040]

[0041] 237.4 g (0.5 mol) Z- L -Ala-NH-C 18 h 37 Add to 1000 mL ethanol, heat to d...

Embodiment 2

[0051] by D Preparation of 4,4'-bithienyl silica with alanine-type cationic surfactant as template.

[0052] The preparation process is the same as in Example 1. In step (1), the raw material Z- L -Ala to Z- D -Ala, keeping other conditions constant.

Embodiment 3

[0054] by L -Phenylglycine-type cationic surfactant as a template for the preparation of 4,4'-bithienyl silica.

[0055] (1) L Synthesis of -16Phg6Et3Br

[0056] 142.6 g ( 0.5 mol ) benzyloxy protected L -Phenylglycine (Z- L -Phg) was dissolved in 400 mL ethyl acetate, and 113.3 g (0.55 mol) DCC was added under ice-water bath, and stirred for 1.0 h. Dissolve 120.7 g ( 0.5 mol ) NH with ethyl acetate 2 (CH 2 ) 15 CH 3 , added to the three-necked flask after cooling, and stirred for 2.0 h. Stir at room temperature for 1.5 h, in an oil bath at 45°C for 48.0 h, and at 60°C for 3.0 h. Add 11.0 mL of glacial acetic acid and continue stirring for 1.0 h. The reaction mixture was filtered while it was hot, and the filtrate was cooled in an ice-water bath. After suction filtration, the solid was collected and recrystallized with n-propanol to obtain the intermediate product Z- L -Phg-NH-C 16 h 37 .

[0057]

[0058] Add 254.4 g ( 0.5 mol ) Z- L -Phg-NH-C 16 h 37 and ...

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PUM

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Abstract

The invention discloses a production method of a spiral bi-thienyl silicon oxide nanometer material, which comprises the following steps that: 1, Z-amino acid and alkylamine form amido linkage through condensation reaction, then a Z protecting group is removed, so an intermediate product A is obtained; 2, the intermediate product A is reacted with bromo acyl chloride to obtain an intermediate product B; 3, the intermediate product B is reacted with triethylamine to obtain an anionic surfactant C; and 4, the spiral bi-thienyl silicon oxide nanometer material is produced by using the anionic surfactant C as a template agent and bi-thienyl silsesquioxane as a silicon source. The production method has a simple process route, easily-obtained raw materials, short reaction time, convenience for operation and no pollution.

Description

[0001] technical field [0002] The invention belongs to the field of nanometer materials, in particular to a method for preparing a helical bithienyl silicon oxide nanometer material. [0003] Background technique [0004] One of the most ubiquitous shapes in nature, the helix is ​​used in DNA and many other tiny structures found in living cells. From galaxies to molecules, asymmetric structures can be seen everywhere. In the field of material preparation, scientists have prepared a variety of chiral and helical nanostructures by using the principle of chiral transfer. Among them, monochiral mesoporous silica nanofibers and nanotubes are the most successful examples. Usually, these nanostructures are prepared by self-assembly of chiral small molecule amphiphiles as templates. These small molecules are generally derivatives of amino acids, glucose or cholesterol. They form monochiral one-dimensional nanofibrous structures through hydrogen bonding, π-π interactions, or s...

Claims

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Application Information

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IPC IPC(8): C01B33/12B82Y40/00B82Y30/00
Inventor 杨永刚李艺李宝宗
Owner 苏州苏凯路化学科技有限公司