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Method using thermo-sensitive segmented copolymer to modify nano-diamond

A nano-diamond and block copolymer technology, applied in the fields of polymer materials and nano-materials, can solve problems such as no nano-microsphere products, and achieve the effects of improving dispersibility, reducing reaction time, and improving temperature sensitivity.

Inactive Publication Date: 2016-09-21
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] However, there are currently no nano-microsphere products prepared by temperature-sensitive block copolymers and nano-diamonds and their published literature and patents.

Method used

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  • Method using thermo-sensitive segmented copolymer to modify nano-diamond
  • Method using thermo-sensitive segmented copolymer to modify nano-diamond

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The preparation of the first step temperature-sensitive block polymer: Add the polyethylene glycol (Mn=2000) of 6.1611g and the stannous octoate of 20mg in the there-necked flask that magnetic stir bar is housed, in N 2 Add 160mL of dry toluene, use a water separation reflux device, heat the oil bath at 130°C (the purpose is to azeotropically remove water from toluene), evaporate about 10mL of toluene, then add 10.6824g of ε-caprolactone with a syringe, and reflux the toluene for 120 ℃ reaction 12h. After the reaction was completed, cool to room temperature, then completely rotate the toluene to evaporate, add 20mL of dichloromethane to dissolve, 200mL of diethyl ether to precipitate, filter with suction, repeat the operation of dichloromethane dissolution-diethyl ether precipitation three times (to purify the product), and dry at 30°C in vacuum. Keep airtight. The obtained product is denoted as PCL-PEG-PCL. The number-average molecular weight of the temperature-sensi...

Embodiment 2

[0042] The first step and the second step are with embodiment 1.

[0043] The third step: take 0.2352g of acidified nano-diamond, 7mL of hexamethylene diisocyanate, 30mL of dry toluene, and ultrasonically disperse at room temperature for 2h, 2 Reaction at 60°C for 24h. After the reaction, wash and filter with dry toluene, repeat the operation 5 times, and dry in vacuum at 60° C. to obtain nanodiamonds with isocyanate functional groups on the surface.

[0044] Step 4: Take 0.0996g of the above-mentioned nano-diamond with isocyanate functional group, 3.0002g of temperature-sensitive block copolymer PCL-PEG-PCL, 50mL of toluene, ultrasonically disperse at room temperature for 2h, and place in N 2 Reaction at 110°C for 48h. After the reaction, wash and filter with dichloromethane, repeat the operation 5 times, and dry in vacuum at 60° C. to obtain nano-diamonds modified by temperature-sensitive block copolymers.

[0045] The average particle diameter of the modified nano-diamon...

Embodiment 3

[0047] The first step and the second step are with embodiment 1.

[0048] Step 3: Take 0.3859g of acidified nano-diamond, 10mL of hexamethylene diisocyanate, 50mL of dry toluene, ultrasonically disperse at room temperature for 2h, and 2 Reaction at 80°C for 12h. After the reaction, wash and filter with dry toluene, repeat the operation 5 times, and dry in vacuum at 60° C. to obtain nanodiamonds with isocyanate functional groups on the surface.

[0049] Step 4: Take 0.1206g of the above-mentioned nano-diamond with isocyanate functional group, 4.0164g of temperature-sensitive block copolymer PCL-PEG-PCL, 60mL of toluene, ultrasonically disperse at room temperature for 2h, and 2 Reaction at 110°C for 72h. After the reaction, wash and filter with dichloromethane, repeat the operation 5 times, and dry under vacuum at 60° C. to obtain nanodiamonds modified by temperature-sensitive block copolymers.

[0050] The average particle diameter of the modified nano-diamond is close to th...

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Abstract

The invention relates to a method using thermo-sensitive segmented copolymer to modify a nano-diamond. The method includes the steps of firstly, preparing the thermo-sensitive segmented copolymer; secondly, preparing the nano-diamond carrying an isocyanate group; thirdly, covalently grafting the thermo-sensitive segmented copolymer to the surface of the nano-diamond. The method has the advantages that the isocyanate group (-NCO) with high reaction activity is used as a connecting bridge, one end of the isocyanate group reacts with the carboxyl (-COOH) and hydroxyl (-OH) on the surface of the nano-diamond, the other end of the isocyanate group reacts with the hydroxyl in the segmented copolymer, and accordingly the thermo-sensitive segmented copolymer with both hydrophilicity and hydrophobicity is grafted to the surface of the nano-diamond, and the nano-diamond is allowed to have good dispersity and stability in both organic solvents and aqueous solvents.

Description

technical field [0001] The invention relates to a method for modifying nano-diamond with a temperature-sensitive block copolymer, which belongs to the technical field of polymer materials and also belongs to the technical field of nano-materials. Background technique [0002] Nanodiamond is a kind of nano inert material with biocompatibility, low toxicity and fluorescence effect. In recent years, nanodiamonds have played an increasingly important role in biomedical fields such as drug carrier materials, biological imaging tools, fluorescent probe materials, and quantum probes. However, due to its ultra-high specific surface area, van der Waals force between particles, electrostatic force, chemical bonding between surface functional groups and many other factors, nano-diamonds are easy to form micron-scale aggregates, which greatly limits the use of nano-diamonds. Applications. Therefore, modifying and deagglomerating nanodiamonds, and exerting its application in biomedicin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L67/04C08K9/04C08K3/04C08G63/08
CPCC08G63/08C08K3/04C08K9/04C08K2201/011C08L2201/06C08L67/04
Inventor 张庆新李文芳于晓燕胡红鑫
Owner HEBEI UNIV OF TECH
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