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Macromolecule cross-linking agent based on oxidized cellulose, gelatin film thereof and preparation method

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

Inactive Publication Date: 2016-01-13
QILU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • Macromolecule cross-linking agent based on oxidized cellulose, gelatin film thereof and preparation method
  • Macromolecule cross-linking agent based on oxidized cellulose, gelatin film thereof and preparation method
  • Macromolecule cross-linking agent based on oxidized cellulose, gelatin film thereof and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

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

[0067] Weigh microcrystalline cellulose (MCC), 2,2,6,6-tetramethylpiperidinyloxy free radical (TEMPO) and NaBr of corresponding quality by mass ratio 400:1:10 in water (80ml / gMCC), During the stirring process, add 5 mmol / g MCC NaClO solution (5% available chlorine) drop by drop, adjust the pH to 10.5, stir magnetically in a water bath at 20°C for 4 hours, centrifuge to collect the precipitate after the reaction, wash with water three times, wash with ethanol once, and vacuum dry at 40°C , to obtain white powdery solid oxidized cellulose TOMCC. 10% (w / v) suspension of TOMCC in water and 0.9g / gTOMCC in NaClO 2 Mixed for secondary oxidation of TOMCC, 5MCH 3 Adjust the pH to 4.2 with COOH, and oxidize for 48 hours. After the oxidation, the precipitate was collected by c...

Embodiment 2

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

[0115] Weigh microcrystalline cellulose (MCC), 2,2,6,6-tetramethylpiperidinyloxy free radical (TEMPO) and NaBr of corresponding quality by mass ratio 400:0.7:8 in water (80ml / gMCC), Add 5 mmol / g MCC NaClO solution (5% available chlorine) drop by drop during stirring, adjust the pH to 10, stir magnetically in a water bath at 20°C for 2 hours, centrifuge to collect the precipitate after the reaction, wash with water three times, wash with ethanol once, and dry in vacuum at 40°C , to obtain white powdery solid oxidized cellulose TOMCC. 10% (w / v) suspension of TOMCC in water and 0.8g / gTOMCC in NaClO 2 Mixed for secondary oxidation of TOMCC, 5MCH 3 Adjust the pH to 4.5 with COOH, and oxidize for 40 hours. After the oxidation, the precipitate was collected by centrifugation, washed three times with water and once with ethanol, and dried in vacuum at 40°C to obtain secondary oxidi...

Embodiment 3

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

[0126] Take microcrystalline cellulose (MCC), 2,2,6,6-tetramethylpiperidinyloxy free radical (TEMPO) and NaBr of corresponding quality by mass ratio 350:1:9 in water (80ml / gMCC), Add 2 mmol / g MCC NaClO solution (available chlorine 5%) drop by drop during the stirring process, adjust the pH to 11, stir magnetically in a water bath at 20°C for 4 hours, centrifuge to collect the precipitate after the reaction, wash with water three times, wash with ethanol once, and vacuum dry at 40°C , to obtain white powdery solid oxidized cellulose TOMCC. 10% (w / v) suspension of TOMCC in water and 0.9g / gTOMCC in NaClO 2 Mixed for secondary oxidation of TOMCC, 5MCH 3 Adjust the pH to 5 with COOH, and oxidize for 48 hours. After the oxidation, the precipitate was collected by centrifugation, washed three times with water and once with ethanol, and dried in vacuum at 40°C to obtain secondary o...

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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 crosslinking agent and gelatin modification, and specifically relates to a macromolecular crosslinking agent based on oxidized cellulose, its gelatin film and a preparation method. Background technique [0002] Gelatin is a heterogeneous peptide molecular polymer produced by the hydrolysis of collagen. It is a natural macromolecule and is widely used in the 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 kind 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, thereby achieving the goal of food industry. ...

Claims

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Application Information

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Patent Type & Authority Applications(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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