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Self-repairing platinum metal gel material, preparation method and application thereof

A technology of gel material and platinum metal, which is applied in the field of self-repairing metal gel materials to achieve excellent laser protection performance, good self-repair performance, and the effect of improving laser protection performance

Active Publication Date: 2021-11-19
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] So far, in the field of laser protection, there are few reports on the use of gel devices to prolong the service life of materials.

Method used

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  • Self-repairing platinum metal gel material, preparation method and application thereof
  • Self-repairing platinum metal gel material, preparation method and application thereof
  • Self-repairing platinum metal gel material, preparation method and application thereof

Examples

Experimental program
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preparation example Construction

[0058] The present invention also provides a preparation method for the compound of formula I, specifically comprising the following steps:

[0059] In a protective atmosphere, compound I and compound II are dissolved in an organic solvent, and a catalyst and an organic base are added to carry out a sonogashira coupling reaction to obtain compound III;

[0060] In a protective atmosphere, compound III and a platinum-containing organometallic reagent undergo a coordination reaction in an organic solvent to form compound IV;

[0061] Compound IV and compound I undergo a sonogashira coupling reaction in an organic solvent under the catalysis of a catalyst to prepare a platinum metal gel material;

[0062] In the above preparation steps, the structural formula of the compound I is

[0063]

[0064] The structural formula of the compound II is

[0065]

[0066] The structural formula of the compound III is

[0067]

[0068] The structural formula of the compound IV is ...

Embodiment 1

[0086] (1) Synthesis of compound 1

[0087]

[0088] 2,7-dibromo-9H-fluorene (15.2g, 45.4mmol, 1eq), bromo-n-hexane (45.4-136.2mmol, 1-3eq), potassium hydroxide (45.4-454mmol, 1-10eq), potassium iodide ( 4.5-45.4mmol, 0.1-1eq) was dissolved in DMSO (80-110eq), and the system was continuously stirred at 0-30°C for 8-12 hours, and the plate was followed to track the reaction. The mixture was diluted with 500eq ethyl acetate, the aqueous phase was separated and extracted again with 100-300eq ethyl acetate. The combined organic phases were dried over anhydrous sodium sulfate and concentrated. The residual solid was purified by silica gel column, and the eluent was petroleum ether and ethyl acetate with a volume ratio of preferably 100:1 to obtain light green oily compound 1 with a yield of 89%. 1 H NMR (400MHz, CDCl 3 ): δ=7.52(d, J=7.7Hz, 2H), 7.46(d, J=6.8Hz, 4H), 1.95–1.87(m, 4H), 1.17–0.97(m, 12H), 0.78(t, J=7.1Hz, 6H), 0.65–0.52(m, 4H).

[0089] (2) Synthesis of compo...

Embodiment 2

[0108] According to the target product Pt-4CHO synthesized in Example 1, in order to test the photophysical properties and self-repairing properties of the target product Pt-4CHO more intuitively and conveniently, the present invention synthesizes the model molecule Pt-4imine on this basis, and the specific synthesis steps are as follows :

[0109]

[0110]Tetraaldehyde platinum complex Pt-4CHO (0.1g, 0.053mmol, 1eq), ethylamine (1-10eq), anhydrous sodium sulfate (1-5eq), in dichloromethane of 200-300eq, under nitrogen React at 20-50°C for 10-30 hours. A red solid was obtained in 90% yield. 1 H NMR (400MHz, CDCl 3 ):δ=10.10(s,2H),10.05(s,2H),9.93(s,2H),8.23(s,2H),7.93–7.90(m,6H),7.87–7.82(m,6H), 7.81–7.73(m,4H),7.72–7.57(m,10H),2.16–1.97(m,16H),1.38–1.20(m,8H),1.20–0.95(m,48H),0.80-0.72(m ,36H), 0.70–0.47(m,16H).

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Abstract

The invention discloses self-repairing platinum metal gel, a preparation method and application thereof, and belongs to the field of self-repairing metal gel materials. The invention relates to a self-repairing platinum metal gel Pt-4CHO, which has a structure as shown in a formula I, and is characterized in that a series of substitution reaction, sonogashira coupling reaction, deprotection reaction and coordination reaction are performed on a raw material 2, 7-dibromo-9H-fluorene, the aldehyde group of Pt-4CHO is converted into an imino group through a Schiff base reaction to synthesize a model molecule Pt-4imine, and systematic research on the performances of photophysics, optical amplitude limiting, self-repairing and the like of the model molecule is carried out. According to the invention, the platinum metal gel prepared by the invention combines an optical amplitude limiting material and a self-repairing gel in a reversible covalent bond form, can be used for researching the optical amplitude limiting performance in a solution state and a gel state while has good self-repairing performance, optical transparency, mechanical property and optical amplitude limiting performance, is excellent in laser protection performance, and is further improved in the laser protection performance due to nonlinear scattering of laser in the gel.

Description

technical field [0001] The invention relates to a self-repairing platinum metal gel material and its preparation method and application, belonging to the field of self-repairing metal gel materials. Background technique [0002] As an important means of modern high-tech warfare, laser technology has been widely used in the military field. With the development of laser technology, the research on corresponding laser protection materials and devices has attracted great attention from all over the world. Among them, the optical limiting material is one of the important materials for laser protection, and its research has extremely important significance. [0003] An ideal optical clipping material would modulate the transmitted intensity of a strong laser beam to a maximum value safe for the desired protection of the optical sensor, but would need to exhibit high transmittance under low-intensity ambient light and should have a linear transmittance High, low clipping threshol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/00B01J13/00
CPCC07F15/0086B01J13/0065
Inventor 刘睿苏欢胡来陈志远朱森强朱红军
Owner NANJING UNIV OF TECH
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