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Cellulose-based guanidine salt bacteriostatic functional material and preparation method thereof

A technology of cellulose-based and functional materials, which is applied in the field of cellulose-based guanidine salt antibacterial functional materials and its preparation, and antibacterial materials, and can solve the problems of unpublished fresh-keeping technology uses, no separation and purification, and unsatisfactory antibacterial effects , achieve good bacteriostasis and biodegradability, simple and convenient operation, and easy processing

Inactive Publication Date: 2014-07-02
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, Chinese patent 200610015785.5 discloses a natural plant spice with antibacterial effect and a preparation method thereof, including 25 kinds of spices such as garlic. The method has more antibacterial components, and some components have unsatisfactory antibacterial effects, and the extract is used , without separation and purification, it has a certain impact on the appearance and smell of fresh fruits and vegetables, but the specific fresh-keeping technology and its specific use have not been announced yet

Method used

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  • Cellulose-based guanidine salt bacteriostatic functional material and preparation method thereof
  • Cellulose-based guanidine salt bacteriostatic functional material and preparation method thereof
  • Cellulose-based guanidine salt bacteriostatic functional material and preparation method thereof

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preparation example Construction

[0040] The preparation method of above-mentioned cellulose-based guanidinium salt antibacterial functional material, comprises the following steps:

[0041] (1) Dissolving cellulose with ionic liquid: When dissolving cellulose with ionic liquid, the temperature is 60-120°C, the stirring time is 6-10 hours, and the mass ratio of ionic liquid to cellulose is 8:1-20:1.

[0042] (2) Modified guanidine salt oligomer: Hexamethylenediamine hydrochloride and amine salt are added to isopropanol or isobutanol, and the mass ratio of hexamethylenediamine hydrochloride and amine salt is (2~7): 1. The synthesis temperature is 120-160°C, the reaction time is 16-24 hours, and the guanidinium salt oligomer is obtained, and then acrylic acid, acrylates or glycidyl methacrylate are added dropwise, wherein acrylic acid, acrylates or methacrylic acid The molar ratio of glycidyl ester to guanidinium salt oligomer is (0.7-1.05):1, the reaction temperature is 80-140°C, and the reaction time is 5-15 h...

Embodiment 1

[0049] Embodiment 1 Preparation of novel cellulose-based guanidine salt antibacterial functional material

[0050] The first step: preparation of guanidinium salt oligomer. Dissolve 11.62g (0.1mol) of hexamethylenediamine in 120ml of isobutanol, adjust the pH to 5-6 with hydrochloric acid; then stand still at -10°C for 12h, filter to leave white crystals, and dry at 60°C for 8h. Obtain 18.3g of hexamethylenediamine hydrochloride, then take 5g of hexamethylenediamine hydrochloride and 1g of dicyandiamide into a 100ml three-necked flask, then add 8.5ml of isopropanol, heat the oil bath to 160°C, stir After 18 hours, an addition reaction was carried out, and 5.5 g of white crystalline guanidinium salt polymer was obtained by cooling.

[0051] The second step: cellulose grafted guanidinium salt.

[0052] a. Weigh 5.5g of white crystalline guanidinium salt polymer, drop into 0.15g of acrylic acid, use the unsaturated double bond in acrylic acid to react with the amino group in gu...

Embodiment 2

[0055] Embodiment 2 Preparation of novel cellulose-based guanidine salt antibacterial functional material

[0056] The first step: preparation of guanidinium salt. Dissolve 11.62g (0.1mol) of hexamethylenediamine in 120ml of isopropanol, adjust the pH to 5-6 with hydrochloric acid; then stand at -10°C for 12h, filter to leave white crystals, and dry at 60°C for 8h. Obtain 18.37g of hexamethylenediamine hydrochloride, then take 8g of hexamethylenediamine hydrochloride and 2g of dicyandiamide into a 100ml three-neck flask, then add 10.5ml of isopropanol, heat the oil bath to 130°C, stir After 18 hours, an addition reaction was carried out, and 9.5 g of white crystalline guanidinium salt polymer was obtained by cooling.

[0057] The second step: cellulose grafted guanidinium salt.

[0058] a. Weigh 9.5g of white crystalline guanidinium salt polymer, drop into 0.25g of acrylic acid, use the unsaturated double bond in acrylic acid to react with the amino group in guanidinium salt...

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Abstract

The invention discloses a cellulose-based guanidine salt bacteriostatic material and a preparation method thereof. The bacteriostatic functional material which is pollution-free, low in cost and naturally degradable is prepared by homogeneously grafting a modified guanidine salt oligomer containing an unsaturated bond to cellulose in ionic liquid. The natural cellulose in the prepared bacteriostatic material is a safe and degradable matrix, the group achieving a bacteriostatic effect is a polymonoguanidine or polydiguanidine repeated unit, the degree of polymerization is 11-19, the cellulose has an excellent inhibiting effect on bacteria and mildew, and the rate of grafting guanidine groups to the cellulose by using the ionic liquid as a homogeneous medium is 15-80%. The prepared cellulose bacteriostatic functional material can be processed into thin films, fibers or other forms and applied in the fields of food and medicine packages, textiles and health products, can inhibit the growth of pathogenic bacteria, and accords with the psychological demands of customers and product manufacturers, so that the cellulose bacteriostatic functional material has great practical application values and economic benefits.

Description

technical field [0001] The invention relates to a bacteriostatic material, in particular to a cellulose-based guanidine salt bacteriostatic functional material and a preparation method thereof, which is especially suitable for the fields of food, pharmaceutical packaging, textiles, hygiene products and the like. Background technique [0002] Cellulose is an environmentally friendly material, which is very rich in nature. Materials based on cellulose not only have good performance and low cost, but also can be biodegraded after use, especially in the face of the current shortage of petroleum resources and the severe environment. question. However, because glucose forms macromolecular polysaccharides, cellulose is insoluble in general solvents, and it is difficult to use directly. Only through special processing or treatment, such as using cuproammonia Cu(NH 3 ) 4 (OH) 2 solution, copper ethylenediamine [NH 2 CH 2 CH 2 NH 2 ]Cu(OH) 2 There are serious environmental pol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G81/00C08G73/00C08B15/06A01N47/44
Inventor 高珊珊王建华张纪娟
Owner QINGDAO UNIV OF SCI & TECH
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