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Preparation method and application of high-molecular weight polyethylene glycol diacrylate (PEGDA)

A technology of polyethylene glycol diacrylate and polyethylene glycol, which is applied in the field of preparation of high molecular weight polyethylene glycol diacrylate (PEGDA), can solve the problems of increased difficulty in PEGDA synthesis and unsuitable synthesis methods, and achieves Good conversion efficiency and reaction effect, simple preparation steps, and enhanced functional effect

Inactive Publication Date: 2014-04-30
广州市一杰医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the influence of steric hindrance, with the increase of molecular weight, the synthesis difficulty of PEGDA will be greatly improved, and the above synthesis method will not be applicable

Method used

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  • Preparation method and application of high-molecular weight polyethylene glycol diacrylate (PEGDA)
  • Preparation method and application of high-molecular weight polyethylene glycol diacrylate (PEGDA)
  • Preparation method and application of high-molecular weight polyethylene glycol diacrylate (PEGDA)

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Experimental program
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Effect test

Embodiment 1

[0063] Embodiment 1: the preparation of PEGDA product

[0064] Add 10g of PEG (molecular weight 3500, sigma, product number P3640) into 150mL of dichloromethane, protect it with argon for 20min, in a water bath at 30°C, add 0.5g of sodium metal, react for 4h to complete the PEG reaction, add 3mL of 25% acrylamide, After 12 hours of reaction, 0.1 g of β-phenylnaphthylamine was added, and vacuum-dried for 24 hours to obtain 11.7 g of PEGDA product.

Embodiment 2

[0065] Embodiment 2: Infrared spectrogram and proton nuclear magnetic resonance spectrum method detect the process of PEGDA product

[0066] Take 1-2 mg of the sample and grind it into a fine powder in an agate mortar, mix it evenly with dry analytically pure potassium bromide powder (about 100 mg, particle size 200 mesh), put it into a mold, and press it into a tablet on a tablet machine. The leaf infrared spectrometer Spectrum65 carried out the spectral measurement of the samples.

[0067] 1H and 13C NMR experimental operation steps, take a small amount of sample into the tube, add 0.5mL deuterated solvent, shake to dissolve the sample, then put the sample into the magnet, open the shimming interface, put the rotor with the sample tube in the Insert above the probe, make the NMR tube enter the probe smoothly, select 1H for test sampling, and select 13C for test sampling in the same operation as above, and obtain 1H and 13C spectra respectively.

[0068] From attached Figu...

Embodiment 3

[0069] Embodiment 3: Gel Permeation Chromatography Determination of PEGDA Molecular Weight

[0070]Select (gel permeation chromatography-multi-angle laser scattering test system (Wyatt Technology, Santa Bar-bara, CA), take a certain amount of 50mg PEGDA and dissolve it in 10mL tetrahydrofuran to prepare a 5mg / mL solution. After overnight, the sample solution passes through the aperture After filtering through a 0.2 μm semi-permeable membrane, inject into the system for measurement. Detection conditions: the mobile phase is chromatographic grade tetrahydrofuran, the flow rate is 0.5mL / min, the temperature is 25°C, and the detector is a multi-angle laser scattering instrument (690nm, DAWN EOS) in conjunction Differential refractometer (690nm Optilab rEX, Wyatt Technology, Santa Barbara, CA), according to the technical report of sigma, the weight-average molecular weight of PEG raw material is 3350, and from the gel permeation chromatography measurement result of PEGDA, the weight...

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Abstract

The invention provides a preparation method of high-molecular weight (greater than 3,000 Dalton) polyethylene glycol diacrylate (PEGDA), which comprises the following steps: fetching high-molecular weight polyethylene glycol (PEG) to react with an organic solvent and an elementary-substance metal; and adding a polymerization inhibitor, and purifying to obtain PEGDA of different yields. According to the method provided by the invention, the high-molecular weight PEG is adopted as a raw material, the use of the reagent with relatively high volatility and toxicity is avoided, the molecular elasticity is improved while the energy consumption is reduced, and the synthesis yield is improved.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a preparation method and application of high molecular weight polyethylene glycol diacrylate (PEGDA). Background technique [0002] Polyethylene glycol (PEG) is non-toxic, non-immunogenic, excellent blood compatibility, and excellent hydrophilicity. It has been approved by the FDA for additives entering the human body and is widely used in pharmaceutical and biomedical materials. middle. Polyethylene glycol diacrylate (PEGDA) is an ideal crosslinking agent for photocrosslinking to form hydrogels or drug-loaded microspheres, and it can also be used as a crosslinking agent for chemical crosslinking. [0003] The Chinese patent with the publication number CN102675562A (application number 201210151477) introduces a high-strength hydrogel cross-linked with polyethylene glycol macromers and its photoinitiated free radical polymerization method, which consists of ...

Claims

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Application Information

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IPC IPC(8): C08G65/48
Inventor 邹学农梁嘉碧周治宇周洪文钟郁
Owner 广州市一杰医药科技有限公司
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