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A kind of preparation method of c18-pmh-peg complex

A technology of C18-PMH-PEG and C18-PMH is applied in the field of preparation of C18-PMH-PEG complexes, which can solve the problem of low yield of RGO-IONP-PEG nano-functional complexes and affect the effective modification of RGO-IONP nano-complexes. , the problem of low compound yield, etc., to shorten the process time, avoid the loss of product yield, and achieve the effect of sufficient reaction

Active Publication Date: 2021-01-26
海南省妇幼保健院
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But when adopting poly(maleic anhydride-1-octadecene) (C18-PMH) and polyethylene glycol (PEG) to carry out grafting reaction at present, the process time required for preparation is longer, and reaction rate is slow, and In the existing preparation method, only about 20% of the carboxyl groups can be effectively connected to PEG, resulting in a low yield of the C18-PMH-PEG complex, which ultimately affects the effective modification of the RGO-IONP nanocomposite, making the resulting RGO -The problem of low yield of IONP-PEG nanofunctional complexes

Method used

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  • A kind of preparation method of c18-pmh-peg complex
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Examples

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Effect test

Embodiment 1-

[0023]Example 1-A preparation method of C18-PMH-PEG complex, including the following steps:

[0024](1) Combine 10mg of poly(maleic anhydride-1-octadecene) (C18-PMH) with 143mgNH2-PEG-OCH3(5k) Mix and dissolve in 5ml dichloromethane solution according to the molar ratio of 1:1. First, ferric chloride and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDC ) Combined as a catalyst, the mass ratio of ferric chloride to 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDC) is 1:3, and the dissolving solution is placed at 80 The catalytic reaction is carried out under microwave radiation at ℃, and the reaction time is 4h under microwave radiation to obtain the initial reaction solution; then 2-(thiophen-2-methyl)phenylboronic acid is added as a catalyst, and the catalytic reaction is continued under microwave radiation at 65℃ 4h, get the reaction solution;

[0025]Wherein, the mass ratio of ferric chloride and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochlorid...

Embodiment 2- 1

[0028]Example 2-A preparation method of C18-PMH-PEG complex, including the following steps:

[0029](1) Combine 10mg of poly(maleic anhydride-1-octadecene) (C18-PMH) with 143mgNH2-PEG-OCH3(5k) Mix and dissolve in 5ml dichloromethane solution according to the molar ratio of 1:1, first use ferrous nitrate and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDC ) Combined as a catalyst, the mass ratio of ferrous nitrate to 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDC) is 1:5, and the dissolving solution is placed at 95 The catalytic reaction was carried out under microwave irradiation at ℃, and the reaction time was 3h under microwave irradiation to obtain the initial reaction liquid; then 2-(thiophen-2-methyl)phenylboronic acid was added as a catalyst, and the catalytic reaction was continued under microwave irradiation at 45℃ 7h, get the reaction solution;

[0030]Wherein, the mass ratio of ferrous nitrate and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide h...

Embodiment 3- 1

[0033]Example 3-A preparation method of C18-PMH-PEG complex, including the following steps:

[0034](1) Combine 10mg of poly(maleic anhydride-1-octadecene) (C18-PMH) with 143mgNH2-PEG-OCH3(5k) Mix and dissolve in 5ml dichloromethane solution according to the molar ratio of 1:1, first use ferrous chloride and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride ( EDC) combined as a catalyst, the mass ratio of ferrous chloride to 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDC) is 1:4, and the solution is placed The catalytic reaction was carried out under microwave irradiation at 85℃, and the reaction time was 4h under microwave irradiation to obtain the initial reaction liquid; then 2-(thiophen-2-methyl)phenylboronic acid was added as a catalyst and continued under microwave irradiation at 55℃ Catalyze the reaction for 5 hours to obtain a reaction liquid;

[0035]Wherein, the mass ratio of ferrous chloride and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochlo...

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Abstract

The present invention provides a kind of preparation method of C18-PMH-PEG composite, comprising: (1) poly(maleic anhydride-1-octadecene) (C18PMH) and NH 2 ‑PEG‑OCH 3 Mix and dissolve in dichloromethane solution, use metal iron salt and EDC as a catalyst, the mass ratio of metal iron salt and EDC is: 1: (3~5), put the solution under microwave radiation at 80~95°C to catalyze the reaction 3-4 hours, to obtain the initial reaction solution; add 2-(thiophene-2-methyl)phenylboronic acid as a catalyst, and catalyze the reaction under microwave radiation at 45-65°C for 4-7 hours, to obtain the reaction solution; (2) the reaction solution Transfer to a constant temperature water bath at 50-65°C, continue to stir at 150-200rpm for 20-35min, take out the solution and blow dry the solution with nitrogen to obtain the crude product solid powder; (3) dissolve the crude product solid powder with deionized water, dialyze for 36-48h, The white powder of C18-PMH-PEG complex is obtained by vacuum freeze-drying at a temperature of -25--30°C; the present invention performs segmented microwave catalytic reactions according to different catalysts, which not only speeds up the reaction rate, but also shortens the time of C18-PMH-PEG The overall process time of the complex was improved, and the yield of the C18‑PMH‑PEG complex was greatly improved.

Description

Technical field[0001]The invention relates to the technical field of composite materials, in particular to a method for preparing a C18-PMH-PEG complex.Background technique[0002]In the existing preparation process of the RGO-IONP-PEG nano-functional composite, polyethylene glycol is usually used to modify the reduced graphene and ferroferric oxide nano-composite (RGO-IONP nano-composite). In order to be able to effectively modify RGO-IONP nanocomposites, usually firstly, the carboxyl groups on poly(maleic anhydride-1-octadecene) (C18-PMH) are directly grafted with polyethylene glycol (PEG) to prepare The amphiphilic C18-PMH-PEG complex is obtained, and then the C18-PMH-PEG complex is ultrasonically mixed with the RGO-IONP nanocomposite for grafting reaction, thereby obtaining the RGO-IONP-PEG nanofunctional complex. However, at present, when poly(maleic anhydride-1-octadecene) (C18-PMH) and polyethylene glycol (PEG) are used for the grafting reaction, the process time required for p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G81/02
CPCC08G81/025
Inventor 战跃福吴烨华王毅翔鲁宏郭子义陈建强关莹
Owner 海南省妇幼保健院
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