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Preparation method of oxidized bacterial cellulose solution

A technology of cellulose solution and bacterial cellulose, which is applied in the field of preparation of oxidized bacterial cellulose solution, can solve the problems of cumbersome operation in the dissolution process, large amount of imidazolyl chloride salt, cumbersome operation process, etc., and achieves outstanding application performance and low system. Viscosity, the effect of a simple dissolution process

Inactive Publication Date: 2018-10-19
TIANJIN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent application number 200910016899.5 of the invention patent "method of dissolving bacterial cellulose" discloses a method of dissolving bacterial cellulose with imidazolium chloride salt ionic liquid.
The patent application No. 200910019950.8 of the invention patent "a method for dissolving bacterial cellulose" discloses that the bacterial cellulose is first activated with ethylenediamine, and then dissolved with lithium chloride / dimethylacetamide mixed liquid. This method operates The process is cumbersome, the amount of medicine is large, and the cost is high

Method used

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  • Preparation method of oxidized bacterial cellulose solution

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Experimental program
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Effect test

Embodiment 1

[0035] (1) The purified bacterial cellulose was mashed with a tissue masher, the rotational speed of the tissue masher was 6000r / min, the tissue mashing time was 20min, and ultrasonication was performed at 400W for 4h.

[0036] (2) Dissolve 0.05mmol / gTEMPO and 0.5mmol / gNaBr (calculated as dry bacterial cellulose) in 100ml distilled water, pour the prepared solution into the homogenate BC obtained from (1), and add 5mmol / g NaClO (in BC dry weight), make the pH of the reaction system remain in the 10.5-11 scope, when the pH value of the reaction system is not changing, 5ml / g terminates the reaction with dehydrated alcohol, can obtain oxidized bacterial cellulose this moment, Wash the obtained oxidized bacterial cellulose with distilled water to neutrality, and the amount of absolute ethanol is 2.5-5ml / g.

[0037] (3) Freeze-dry the oxidized bacterial cellulose obtained in (2), and re-grind into powder with a pulverizer, and the speed of the pulverizer is 15000r / min.

[0038] (4...

Embodiment 2

[0042] (1) The purified bacterial cellulose was mashed with a tissue masher, the rotation speed of the tissue masher was 8000r / min, the tissue mashing time was 15min, and ultrasonication was performed at 1000W for 30min.

[0043] (2) Dissolve 0.05mmol / gTEMPO and 1mmol / gNaBr (in BC dry weight) in 100ml distilled water, pour the prepared solution into the homogenate BC obtained in (1), and add 10mmol / g NaClO (in BC dry weight) BC dry weight), keep the pH of the reaction system in the range of 10.5-11, when the pH value of the reaction system is not changing, stop the reaction with absolute ethanol at 5ml / g, at this time, oxidized bacterial cellulose can be obtained, and use distilled water The obtained oxidized bacterial cellulose is washed to neutrality, and the amount of absolute ethanol is 5-6ml / g.

[0044] (3) Blast-dry the oxidized bacterial cellulose obtained in (2), and re-grind into powder with a pulverizer, and the pulverizer speed is 15000r / min.

[0045] (4) Prepare a...

Embodiment 3

[0049] (1) The purified bacterial cellulose was mashed with a tissue masher, the rotation speed of the tissue masher was 12000r / min, the tissue mashing time was 10min, and ultrasonication was performed at 800W for 1h.

[0050] (2) Dissolve 0.1mmol / gTEMPO and 1mmol / gNaBr (in BC dry weight) in 100ml distilled water, pour the prepared solution into the homogenate BC obtained in (1), and add 10mmol / g NaClO (in BC dry weight) BC dry weight), keep the pH of the reaction system in the range of 10.5-11, when the pH value of the reaction system is not changing, stop the reaction with absolute ethanol at 5ml / g, at this time, oxidized bacterial cellulose can be obtained, and use distilled water The obtained oxidized bacterial cellulose is washed to neutrality, and the amount of absolute ethanol is 5-8ml / g.

[0051] (3) Naturally air-dry the oxidized bacterial cellulose obtained in (2), and re-grind into powder with a pulverizer, and the speed of the pulverizer is 18000r / min.

[0052] (4...

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Abstract

The invention discloses a preparation method of an oxidized bacterial cellulose solution, and belongs to the field of dissolution of bacterial cellulose. The preparation method comprises the followingsteps: purifying, crushing, homogenizing and performing ultrasonic treatment to bacterial cellulose, then oxidizing by a mixed oxidizing system of TEMPO / NaBr / NaClO, then washing, performing dry crushing or dewatering to obtain oxidized bacterial cellulose powder or an oxidized bacterial cellulose slurry, dissolving the oxidized bacterial cellulose powder or the oxidized bacterial cellulose slurryby using an aqueous alkaline dissolving agent solution, then standing at a low temperature for freezing, and thawing to obtain the transparent oxidized bacterial cellulose solution. The preparation method is simple and easy to implement, a technology is easy to control, the reagent dosage is relatively low, and the cost is saved; by the preparation method, the cellulose can be effectively dissolved to directly obtain the oxidized bacterial cellulose solution; the oxidized bacterial cellulose solution can be widely applied to the field of packaging, biomedical materials, intelligent hydrogels,membrane preparation, preparation of specially-shaped hydrogels and the like, so that the application field of the bacterial cellulose is widened.

Description

technical field [0001] The invention belongs to the field of bacterial cellulose dissolution, and in particular relates to a preparation method of an oxidized bacterial cellulose solution. Background technique [0002] Bacterial cellulose is a kind of degradable material. Compared with plant cellulose, bacterial cellulose has the advantages of higher chemical purity, fast synthesis speed, and controllable synthesis process. However, bacterial cellulose has high crystallinity, polymerization Degree and intramolecular hydrogen bond and intermolecular hydrogen bond, which makes bacterial cellulose difficult to dissolve. At present, the development of new cellulose green solvents and processes has become an important direction for the development of the cellulose industry. [0003] At present, with the advancement of science and technology and the emphasis on health in human society, smart biomaterials that can respond to changes in external environmental conditions have become ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B15/02C08J3/05C08L1/04
CPCC08B15/02C08J3/05C08J2301/04
Inventor 钟成李博贾士儒谢燕燕刘其敬谭之磊韩培培
Owner TIANJIN UNIV OF SCI & TECH
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