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A kind of preparation method of hydrophobically modified cellulose polymer micelles

A technology of cellulose polymer and hydrophobic modification, which is applied in the field of preparation of hydrophobically modified cellulose polymer micelles, can solve the problems of limited method of amphiphilic polymer, complicated reaction, difficult product handling, etc., and achieves good storage. Effects of Stability and Dilution Stability

Active Publication Date: 2021-03-19
SHAANXI UNIV OF SCI & TECH
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  • Description
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  • Application Information

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Problems solved by technology

However, the construction of these self-assembled supramolecular structures is mostly aimed at water-soluble cellulose derivatives. In addition to expensive solvents, a large amount of organic solvents, Heavy metal catalysts and petroleum-based monomers lead to complex reactions and difficult product handling; while in green solvents, the methods for preparing amphiphilic polymers of cellulose bulk are very limited, and there is no research on hydrophobic long-chain alkylated cellulose gelatin Report on the preparation method of polymer

Method used

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  • A kind of preparation method of hydrophobically modified cellulose polymer micelles
  • A kind of preparation method of hydrophobically modified cellulose polymer micelles
  • A kind of preparation method of hydrophobically modified cellulose polymer micelles

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preparation example Construction

[0035] The invention provides a method for preparing hydrophobically modified cellulose polymer micelles, a method for preparing hydrophobically modified cellulose polymer micelles, comprising the following specific steps:

[0036] Step 1, weighing raw materials:

[0037] Step 2, prepare cellulose solution:

[0038] Adding the weighed sodium hydroxide and urea into water in sequence to obtain a mixed solution of sodium hydroxide and urea, precooling; then throwing in cellulose, and stirring the obtained cellulose solution;

[0039] Step 3, preparation of cellulose gelatin polymer:

[0040] Add gelatin aqueous solution dropwise to the cellulose solution, stir at room temperature for 1 hour, add epichlorohydrin while stirring, react for 3 to 5 hours, undergo dialysis, dispersion, standing, and separation to obtain a water-soluble cellulose gelatin polymer;

[0041] Step 4, preparation of hydrophobically modified cellulose polymer:

[0042] Add brominated long-chain alkyl grou...

Embodiment 1

[0060]Dissolve 2 g of cellulose in 98 g of sodium hydroxide and urea mixed solution precooled to -12°C to obtain a cellulose solution; add 2.78 g of an 8% gelatin aqueous solution dropwise to the cellulose solution, and stir at room temperature for 1 h. Subsequently, 6 g of epichlorohydrin was added dropwise, the reaction was continued for 3 h, and then the water-soluble cellulose gelatin polymer was obtained through dialysis, dispersion, standing, and separation;

[0061] Weigh 20g of cellulose gelatin polymer aqueous solution in a 100mL three-necked flask, adjust the pH of the system to 11, add n-octane bromide dropwise, wherein the molar ratio of n-octane bromide to cellulose glucose unit is 6:1, and control the reaction The temperature is 40°C, stirred for 8 hours, stopped the reaction, neutralized with hydrochloric acid, and after the system temperature dropped to room temperature, the reaction product was precipitated with absolute ethanol and washed 3 times, and vacuum-d...

Embodiment 2

[0067] Dissolve 3 g of cellulose in 97 g of sodium hydroxide and urea mixed solution precooled to -11°C to obtain a cellulose solution; add 8.82 g of an aqueous gelatin solution with a mass fraction of 8.5% to the cellulose solution dropwise, and stir at room temperature for 1 h. Subsequently, 7.5 g of epichlorohydrin was added dropwise, and the reaction was continued for 3.5 h, followed by dialysis, dispersion, standing, and separation to obtain a water-soluble cellulose gelatin polymer;

[0068] Weigh 20g of cellulose gelatin polymer aqueous solution in a 100mL three-neck flask, adjust the pH of the system to 12, add bromododecane dropwise, wherein the molar ratio of bromododecane to cellulose glucose unit is 8:1, and control the reaction The temperature is 50°C, stirred for 7 hours, stopped the reaction, neutralized with hydrochloric acid, and after the system temperature dropped to room temperature, the reaction product was precipitated with absolute ethanol and washed 4 ti...

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Abstract

The invention discloses a preparation method of a hydrophobically modified cellulose polymer micelle. The preparation method comprises the following specific steps: step 1, weighing raw materials; step 2, preparing a cellulose solution; step 3, preparing a cellulose gelatin polymer; 4, preparing a hydrophobically modified cellulose polymer; and step 5, preparing the hydrophobically modified cellulose polymer micelle. Cellulose is dissolved in a mixed solution of sodium hydroxide and urea and is subjected to coupling copolymerization with gelatin and epichlorohydrin, and the water-soluble cellulose gelatin polymer is obtained through dialysis, dispersing, standing and separation; and then a brominated long-chain alkyl group is added into the cellulose gelatin polymer, the pH value of the system is adjusted, and the solution is stirred for a reaction, neutralized with hydrochloric acid, cooled to room temperature, precipitated with absolute ethanol, washed repeatedly, and dried in vacuumto obtain the hydrophobically modified cellulose polymer; and the hydrophobically modified cellulose polymer is dialyzed to obtain the hydrophobically modified cellulose polymer micelle. The particlesize of the prepared hydrophobically modified cellulose polymer micelle is 104-806 nm and the critical micelle concentration is 0.135-0.628 mg / mL.

Description

technical field [0001] The invention belongs to the technical field of polymer material preparation, and relates to a method for preparing hydrophobically modified cellulose polymer micelles. Background technique [0002] As we all know, self-assembly technology is one of the most promising strategies to realize amphiphilic polymer micelles; thermodynamically Stable, structurally specific three-dimensional supramolecular structures. The molecular structure of amphiphilic block copolymers contains hydrophilic and hydrophobic segments, which can self-assemble into micelles with different shapes in aqueous solution, and have potential applications in the fields of drug controlled release, biosensors, bioimaging and fluorescent probes. application value. However, the preparation of self-assembled micelles based on synthetic block copolymers has disadvantages such as high cost, high pollution, non-renewability, and potential biotoxicity. In order to overcome these shortcomings...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B15/00C08J3/05
CPCC08B15/00C08J3/05C08J2301/02
Inventor 王鸿儒姚一军柴雍王瑞瑞
Owner SHAANXI UNIV OF SCI & TECH
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