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Macromolecular crosslinking agent based on oxidized cellulose, its gelatin film and preparation method

A technology of macromolecular cross-linking agent and oxidized cellulose, which is applied in the direction of climate change adaptation, sustainable manufacturing/processing, flexible coverings, etc., can solve the problems of low light transmittance and low transparency of gelatin film, and achieve mechanical properties Good, the effect of improving hydrophobicity and maintaining light-blocking properties

Inactive Publication Date: 2017-11-07
QILU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

And the light transmittance of the prepared gelatin film is low, resulting in its low transparency, which is very unfavorable for food packaging materials.
In addition, gelatin film has certain limitations in anti-degradation utilization
[0005] There are few studies on the modification of gelatin film by oxidized fiber-based active esters. For the oxidation of cellulose with 2,2,6,6-tetramethylpiperidine nitroxide radical (TEMPO) / NaBr / NaClO, and then N -Hydroxysuccinimide activates oxidized cellulose to form active ester TMN modified gelatin film and the patent research on its biodegradation mechanism has not been reported

Method used

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  • Macromolecular crosslinking agent based on oxidized cellulose, its gelatin film and preparation method
  • Macromolecular crosslinking agent based on oxidized cellulose, its gelatin film and preparation method
  • Macromolecular crosslinking agent based on oxidized cellulose, its gelatin film and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0065] A synthetic method of a novel macromolecular cross-linking agent based on oxidized cellulose:

[0066] (1) Preparation of oxidized cellulose (TOMCC) and determination of carboxyl aldehyde group content:

[0067] Weigh the corresponding mass of microcrystalline cellulose (MCC), 2,2,6,6-tetramethylpiperidinyloxy radical (TEMPO) and NaBr in water (80ml / g MCC) in a mass ratio of 400:1:10. , 5mmol / g MCC's NaClO solution (5% available chlorine) was added dropwise during stirring, the pH was adjusted to 10.5, and the water bath was magnetically stirred for 4h at 20°C. Vacuum drying yielded a white powdery solid oxidized cellulose TOMCC. 10% (w / v) suspension of TOMCC in water with 0.9 g / g TOMCC in NaClO 2 Mixed secondary oxidation of TOMCC, 5M CH 3 The pH was adjusted to 4.2 with COOH, and oxidized for 48 h. After the oxidation, the precipitate was collected by centrifugation, washed with water three times, washed with ethanol once, and dried in vacuum at 40°C to obtain seco...

Embodiment 2

[0114] (1) Preparation of oxidized cellulose (TOMCC) and determination of carboxyl aldehyde group content:

[0115]Weigh the corresponding mass of microcrystalline cellulose (MCC), 2,2,6,6-tetramethylpiperidinyloxy radical (TEMPO) and NaBr in water (80ml / g MCC) in a mass ratio of 400:0.7:8 , 5mmol / g MCC NaClO solution (available chlorine 5%) was added dropwise during the stirring process, the pH was adjusted to 10, and the water bath was magnetically stirred for 2h at 20°C. Vacuum drying yielded a white powdery solid oxidized cellulose TOMCC. 10% (w / v) suspension of TOMCC in water with 0.8 g / g TOMCC in NaClO 2 Mixed secondary oxidation of TOMCC, 5M CH 3 The pH was adjusted to 4.5 with COOH, and oxidized for 40 h. After the oxidation, the precipitate was collected by centrifugation, washed with water three times, washed with ethanol once, and vacuum-dried at 40 °C to obtain secondary oxidized cellulose. The carboxyl group content of TOMCC and the aldehyde group content of se...

Embodiment 3

[0125] (1) Preparation of oxidized cellulose (TOMCC) and determination of carboxyl aldehyde group content:

[0126] Weigh the corresponding mass of microcrystalline cellulose (MCC), 2,2,6,6-tetramethylpiperidinyloxy radical (TEMPO) and NaBr in water (80ml / g MCC) in a mass ratio of 350:1:9 , 2mmol / g MCC NaClO solution (5% available chlorine) was added dropwise during stirring, pH was adjusted to 11, magnetic stirring was performed in a water bath at 20°C for 4h, after the reaction was completed, the precipitate was collected by centrifugation, washed with water three times, washed with ethanol once, at 40°C Vacuum drying yielded a white powdery solid oxidized cellulose TOMCC. 10% (w / v) suspension of TOMCC in water with 0.9 g / g TOMCC in NaClO 2 Mixed secondary oxidation of TOMCC, 5M CH 3 The pH was adjusted to 5 with COOH, and oxidized for 48 h. After the oxidation, the precipitate was collected by centrifugation, washed with water three times, washed with ethanol once, and va...

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Abstract

The invention discloses a macromolecule cross-linking agent based on oxidized cellulose, a gelatin film thereof and a preparation method. The preparation method of the gelatin film comprises the following steps: 1, oxidizing a primary amino group on the C6 position of cellulose into carboxyl through a TEMPO / NaBr / NaClO system, and obtaining oxidized cellulose TOMCC; 2, treating N-hydroxy succinimide and TOMCC obtained in step 1 as raw materials, and manufacturing a macromolecule cross-linking agent TMN; 3, making the macromolecule cross-linking agent TMN be subjected to chemical cross-linking with a gelatin film, and obtaining the food package gelatin film based on oxidized cellulose chemical cross-linking. Light-blocking performance, thermal stability, anti-biodegradation capability, the mechanical property (elasticity) and hydrophobicity of the gelatin film are all improved to a large extent, and a favorable condition is provided for application of the gelatin film to the food package field. In addition, biodegradation mechanisms of a modified gelatin film and a pure gelatin film in a phosphate buffered solution (PBS) and lysozyme are explored and analyzed as well.

Description

technical field [0001] The invention belongs to the field of macromolecular cross-linking agent and gelatin modification, and particularly relates to a macromolecular cross-linking agent based on oxidized cellulose, a gelatin film thereof and a preparation method. Background technique [0002] Gelatin is a non-uniform peptide molecular polymer produced by collagen hydrolysis. It is a natural macromolecule. It is widely used in food industry and other fields because of its non-toxic and good physical and chemical properties. However, its low thermal stability, poor mechanical properties, and easy degradation limit its application, so gelatin is often modified. [0003] Microcrystalline cellulose (MCC) is a type of linear polysaccharide macromolecular structure connected by β-glycosidic bonds. It is often blended with gelatin or the characteristic functional groups obtained after oxidation react with gelatin to modify gelatin, and then achieve the goal of food industry. Requi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B15/06C08J5/18C08J3/24C08L89/00C08L1/08C08K5/053B65D65/38
CPCY02A40/90Y02W90/10
Inventor 崔月芝庄辰陶芙蓉
Owner QILU UNIV OF TECH
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