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Cellulose based macromolecular cross-linking agent, preparation method thereof and application of cellulose based macromolecular cross-linking agent in preparation of modified gelatin

A technology of macromolecular cross-linking agent and cellulose, which is applied in the application field of making modified gelatin to achieve the effect of improving light blocking performance and hydrophobicity

Inactive Publication Date: 2015-08-26
QILU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, there are very few studies on the use of fiber-based active esters to modify gelatin films. There is still a lack of patent research on functionalizing cellulose with EDTAD and then activating functional cellulose with N-hydroxysuccinimide to form active esters MEN modified gelatin films. No report

Method used

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  • Cellulose based macromolecular cross-linking agent, preparation method thereof and application of cellulose based macromolecular cross-linking agent in preparation of modified gelatin
  • Cellulose based macromolecular cross-linking agent, preparation method thereof and application of cellulose based macromolecular cross-linking agent in preparation of modified gelatin
  • Cellulose based macromolecular cross-linking agent, preparation method thereof and application of cellulose based macromolecular cross-linking agent in preparation of modified gelatin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] A kind of synthetic method of novel macromolecular cross-linking agent based on cellulose:

[0050] (1) Synthesis of EDTA dianhydride (EDTAD):

[0051]Weigh 20 g of EDTA disodium salt and dissolve it in 100 ml of water to form a transparent solution, add 1.5 mol / L HCl dropwise during stirring until a white precipitate appears, and filter with suction to obtain EDTA; weigh 18 g of EDTA and 24 ml of acetic anhydride in Suspension was formed in 31 ml of pyridine, magnetically stirred in an oil bath at 65 °C for 24 h, after the reaction was completed, it was washed with distilled water and ether, then suction filtered, and vacuum-dried at 50 °C to obtain white powdery solid EDTA dianhydride (EDTAD).

[0052] Such as figure 1 Shown, 1H NMR (400MHz, DMSO): δ 3.691 (s, 8H), 2.657 (s, 4H), 3.08 (s, DMSO), 2.496-2.488 (m, DMSO).

[0053] (2) Preparation of EDTAD functionalized microcrystalline cellulose (ME):

[0054] Weigh 3 g of microcrystalline cellulose (MCC) and 9 g of E...

Embodiment 2

[0072] (1) Synthesis of EDTA dianhydride (EDTAD):

[0073] Weigh 30 g of EDTA disodium salt and dissolve it in 150 ml of water to form a transparent solution, add 1 mol / L HCl dropwise during stirring until a white precipitate appears, and filter with suction to obtain EDTA; weigh 21 g of EDTA and 30 ml of acetic anhydride in Suspension was formed in 40 ml of pyridine, magnetically stirred in an oil bath at 72 °C for 24 h, after the reaction was completed, it was washed with distilled water and then with diethyl ether, then vacuum-dried at 50 °C to obtain white powdery solid EDTA dianhydride (EDTAD).

[0074] (2) Preparation of EDTAD functionalized microcrystalline cellulose (ME):

[0075] Weigh 3 g of MCC and 12 g of EDTAD in 150 ml of DMF, and stir magnetically in an oil bath at 73°C for 30 h. Suction filtration after washing, and vacuum drying at 50°C to obtain a light yellow powdery solid compound, namely, EDTAD functionalized microcrystalline cellulose ME;

[0076] (3) P...

Embodiment 3

[0079] (1) Synthesis of EDTA dianhydride (EDTAD):

[0080] Weigh 40 g of EDTA disodium salt and dissolve it in 200 ml of water to form a transparent solution, add 2 mol / L HCl dropwise during the stirring process until a white precipitate appears, and filter to obtain EDTA; weigh 25 g of EDTA and 40 ml of acetic anhydride in Suspension was formed in 50 ml of pyridine, magnetically stirred in an oil bath at 75 °C for 36 h, after the reaction was completed, it was washed with distilled water and then with ether, then suction filtered, and vacuum-dried at 50 °C to obtain white powdery solid EDTA dianhydride (EDTAD).

[0081] (2) Preparation of EDTAD functionalized microcrystalline cellulose (ME):

[0082] Weigh 3 g of MCC and 10 g of EDTAD in 120 ml of DMF, and stir magnetically in an oil bath at 65 °C for 20 h. Suction filtration after washing, and vacuum drying at 50°C to obtain a light yellow powdery solid compound, namely, EDTAD functionalized microcrystalline cellulose ME; ...

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Abstract

The invention discloses a cellulose based macromolecular cross-linking agent, a preparation method thereof and an application of the cellulose based macromolecular cross-linking agent in preparation of modified gelatin, and belongs to the field of gelatin cross-linking agents. The preparation method of the cross-linking agent comprises steps as follows: 1), EDTA (ethylene diamine tetraacetic acid) dianhydride and microcrystalline cellulose are taken as raw materials to prepare EDTA dianhydride functionalized microcrystalline cellulose ME; 2), N- hydroxysuccinimide and ME obtained in the step 1) are taken as raw materials to prepare the macromolecular cross-linking agent. The ester group in the cross-linking agent can have a cross-linking reaction with primary amino in gelatin, a gelatin film is modified in a chemical reaction manner, and the limitation of gelatin modification through cellulose macromolecule blending in the prior art is broken. The heat stability, the degradation resistance, the mechanical property (elasticity), the light blocking performance and the hydrophobicity of the gelatin film are improved to a greater degree.

Description

technical field [0001] The invention relates to the field of macromolecular crosslinking agents, in particular to a novel cellulose-based macromolecular crosslinking agent, its preparation method and its application in making modified gelatin. Background technique [0002] Gelatin is a heterogeneous peptide molecular polymer produced by the hydrolysis of collagen. It is a natural polymer material with good cell compatibility and biodegradability. However, its application is limited due to its low thermal stability, poor mechanical properties, and easy degradation. Therefore, gelatin is often modified. [0003] Microcrystalline cellulose (MCC) is a kind of linear polysaccharide macromolecular structure connected by b-glycosidic bonds, and gelatin is often modified by blending. For example, Alves studied the effect of cellulose content on the biodegradability, mechanical properties and moisture permeability of gelatin / cellulose / starch blend films (J.S. Alves, K.C. dos Reis, E...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B15/06C08H1/00C08J5/18
Inventor 陶芙蓉庄辰崔月芝
Owner QILU UNIV OF TECH
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