CN104558212B - Application of aminated bio-cellulose to preparation of moist dressing - Google Patents
Application of aminated bio-cellulose to preparation of moist dressing Download PDFInfo
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- CN104558212B CN104558212B CN201510043319.7A CN201510043319A CN104558212B CN 104558212 B CN104558212 B CN 104558212B CN 201510043319 A CN201510043319 A CN 201510043319A CN 104558212 B CN104558212 B CN 104558212B
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Abstract
The invention relates to a preparation method of aminated bio-cellulose. The method comprises the steps of reacting bio-cellulose with epoxy chloropropane in an alkaline solution and reacting the reacted bio-cellulose with ammonia water in a weak alkaline solution. The method is simple and convenient in operation and low in cost; and when the produced aminated bio-cellulose is in contact with nano metal particles, the firmness degree of combination in a chelating form can be improved, and the stability and the safety of the bio-cellulose nano metal particle composite material can be improved.
Description
Technical field
The present invention relates to the technical field of modification to the biology cellulose as " moist dressing " material, especially relate to one
Plant the preparation method of amination biology cellulose.
Background technology
Biology cellulose（biocellulose）It is the fiber element being produced by metabolism by certain micro-organisms.Due to it
In there is excellent space net structure, therefore it has special physicochemical form, and such as it has stronger mechanical performance,
Good water holding, water retention property, good biocompatibility and biodegradability.It is by initially answering in field of food
With slowly developing into the application in biomedicine field, it is with a wide range of applications as " moist dressing " at present.
Biology cellulose-nanometer silver composite wood is individually disclosed in Chinese patent CN102212806A, CN102206355A
The preparation method of material and the preparation method of the biological cellulose membrane containing nanometer silver, although concrete grammar is different, it is all profit
With biology cellulose, nano-silver ionic is adsorbed thereon, and improve it as the anti-microbial property of " moist dressing ".But, due to life
Fibres element film and nanoparticle between adhesion relatively weak so that adsorbed silver ion is in follow-up processing or use
In easily from the landing of film surface, not only affect the anti-microbial property of product, serious if also human body can be worked the mischief.Therefore,
A kind of method of biology cellulose selectivity amination is disclosed, it has carried out amination to biology cellulose in CN102276736A,
Produce amino, using the combination of amino and metallic element particle sequestration form, provide and more firmly combine compared with coordinate bond.
But, the method sufficiently complex it is necessary first to lyophilization is carried out to Bacterial cellulose, its requirement to process equipment, cost
All very high, the plurality of raw materials such as nitroxyl compound also to be used, enzyme, diamine compounds thereafter, need through complexity
Step is processed, and is unfavorable for large-scale application.
Content of the invention
For drawbacks described above, the present invention provides a kind of preparation method of new amination biology cellulose, its simple to operate, one-tenth
This is cheap, and is obtained in that the respond well amination biology cellulose product of amination.
The preparation method of the amination biology cellulose that the present invention provides, it comprises the steps：
（1）Make biology cellulose in alkaline solution, with epichlorohydrin reaction；
（2）Make, in reacted biology cellulose weakly alkaline solution, to react with ammonia.
In said method, described biology cellulose is undried biology cellulose wet film；
In said method, step（1）In alkaline solution pH value more than 12, its consumption is that 300-500 ml/g is biological
Cellulose, preferably described alkaline solution is the sodium hydroxide solution of 1mol/L, and consumption is 400.
In said method, step（1）The consumption of middle epoxychloropropane is 10-30mmol/g biology cellulose, preferably 15-
20mmol/g biology cellulose.
In said method, step（1）Biology cellulose is 50-80 DEG C with the temperature conditionss of epichlorohydrin reaction, preferably
60℃；Response time 1-4 hour, preferably 2 hours.
In said method, step（2）In alkaline solution pH value below 12, its consumption be 300-500ml/g life
Fibres element, preferably described alkaline solution is the sodium hydroxide solution of 0.01mol/L, and consumption is 400ml/g biology cellulose.
In said method, step（2）The concentration of middle ammonia is 20-30%, and consumption is 10-20ml/g biology cellulose, preferably
Concentration is the ammonia of 25-28%, and consumption is 12-16ml/g biology cellulose.
In said method, step（2）The temperature conditionss that biology cellulose and ammonia react are 50-80 DEG C, preferably 60 DEG C；Instead
1-4 hour between seasonable, preferably 2 hours.
In said method, preferably in step（1）After end, there is taking-up biology cellulose, be washed with distilled water to pH value fall
Low to 12 below step.
In said method, preferably in step（2）After end, there is taking-up biology cellulose, be washed with distilled water to neutrality
Step.
Specifically, the invention provides a kind of preparation method of amination biology cellulose, it comprises the steps：
（1）Take biology cellulose, add the sodium hydroxide of 1M molten in the volume mass of ml/g than the ratio for 300-500
Liquid, heats while stirring, and to when being warmed up to 50-80 DEG C, the ratio according to 10-30mmol/g biology cellulose adds epoxy chloropropionate
Alkane, keeping temperature reacts 1-4 hour；
（2）Take out biology cellulose, be washed with distilled water to pH value and be reduced to less than 12；
（3）Add the hydroxide of 0.01M in the volume mass of ml/g than the ratio for 300-500 in biology cellulose again
Sodium solution, heats while stirring, and to when being warmed up to 50-80 DEG C, addition concentration is 20-30% ammonia, and addition is 10-20ml/g
Biology cellulose, insulation reaction 1-4 hour；
（4）Take out biology cellulose, be washed with distilled water to neutrality.
In said method, step（1）The volume of the sodium hydroxide solution of the 1M of middle addition is the 400 of biology cellulose quality
Times；
In said method, step（1）Temperature when middle epoxychloropropane adds is 60 DEG C, and the temperature of insulation reaction is also 60
DEG C, the response time is 2 hours；
In said method, step（1）The addition of middle epoxychloropropane is 18mmol/g biology cellulose；
In said method, step（3）The volume of the sodium hydroxide solution of the 0.011M of middle addition is biology cellulose quality
400 times；
In said method, step（3）Temperature when middle ammonia adds is 60 DEG C, and the temperature of insulation reaction is also 60 DEG C, instead
It is 2 hours between seasonable；
In said method, step（3）The concentration of middle ammonia is 25-28%, and consumption is 12-16ml/g biology cellulose.
The present invention also offer amination biology cellulose of method preparation in the present invention contains nano-metal particle in preparation
Purposes in composite.
Using the method for the present invention, easy and simple to handle, with low cost, and produce the biology cellulose of amination, its with receive
During rice metallic particles contact, the combination of sequestration form can be passed through, improve the firmness combining, improve biology cellulose nanometer
The stability of metal particle composite media and safety.
Specific embodiment
With reference to specific embodiment and contrast experiment, the present invention is further illustrated, but tool hereinafter
Body implementation is understood not to limitation of the present invention.Those of ordinary skill in the art can show on the basis of the present invention
And the various changes that easy insight is made and change are it should all within the scope of the present invention.
Embodiment 1
Take biology cellulose 0.1g, add the sodium hydroxide solution 40ml of 1M, heat while stirring, to being warmed up to 50 DEG C
When, add the epoxychloropropane of 1.5mmol, keeping temperature is reacted 2 hours, take out biology cellulose, be washed with distilled water to pH
It is worth for 11；Add the sodium hydroxide solution 35ml of 0.01M again in biology cellulose, heat while stirring, to being warmed up to 60 DEG C
When, addition 1.2ml concentration is 28% ammonia, and insulation reaction 2 hours is taken out biology cellulose, is washed with distilled water to neutrality, system
Obtain the amination biology cellulose of the present invention.
Embodiment 2
Take biology cellulose 0.1g, add the sodium hydroxide solution 30ml of 1M, heat while stirring, to being warmed up to 70 DEG C
When, add the epoxychloropropane of 1.8mmol, keeping temperature is reacted 2 hours, take out biology cellulose, be washed with distilled water to pH
It is worth for 10；Add the sodium hydroxide solution 55ml of 0.01M again in biology cellulose, heat while stirring, to being warmed up to 60 DEG C
When, addition 1.5ml concentration is 25% ammonia, and insulation reaction 2 hours is taken out biology cellulose, is washed with distilled water to neutrality, system
Obtain the amination biology cellulose of the present invention.
Embodiment 3
Take biology cellulose 1g, add the sodium hydroxide solution 400ml of 1M, heat while stirring, to when being warmed up to 60 DEG C,
Add the epoxychloropropane of 19mmol, keeping temperature is reacted 2 hours, take out biology cellulose, being washed with distilled water to pH value is
10；Add the sodium hydroxide solution 400ml of 0.01M again in biology cellulose, heat while stirring, to when being warmed up to 60 DEG C,
Addition 16ml concentration is 27% ammonia, and insulation reaction 2 hours is taken out biology cellulose, is washed with distilled water to neutrality, and this is obtained
The amination biology cellulose of invention.
Embodiment described above is only that the preferred embodiment of the present invention is described, the not model to the present invention
Enclose and be defined, on the premise of without departing from design spirit of the present invention, the skill to the present invention for this area ordinary skill technical staff
Various modifications and improvement that art scheme is made, all should fall in the protection domain of claims of the present invention determination.
Claims (1)
1. a kind of amination biology cellulose preparation the moist dressing material containing nano-Ag particles in purposes it is characterised in that
Described amination biology cellulose is by the method preparation comprising the steps：
（1）Take biology cellulose, add the sodium hydroxide solution of 1M in the ratio of 300-500ml/g biology cellulose, side is heated
Side is stirred, and to when being warmed up to 50-80 DEG C, the ratio according to 10-30mmol/g biology cellulose adds epoxychloropropane, keeps temperature
Degree reaction 1-4 hour；
（2）Take out biology cellulose, be washed with distilled water to pH value and be reduced to less than 12；
（3）Add the sodium hydroxide solution of 0.01M in the ratio of 300-500ml/g biology cellulose in biology cellulose again,
Heat while stirring, to when being warmed up to 50-80 DEG C, addition concentration is 20-30% ammonia, and addition is 10-20ml/g biological fiber
Element, insulation reaction 1-4 hour；
（4）Take out biology cellulose, be washed with distilled water to neutrality；
Wherein said biology cellulose is undried biology cellulose wet film.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510043319.7A CN104558212B (en) | 2015-01-29 | 2015-01-29 | Application of aminated bio-cellulose to preparation of moist dressing |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510043319.7A CN104558212B (en) | 2015-01-29 | 2015-01-29 | Application of aminated bio-cellulose to preparation of moist dressing |
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| CN104558212A CN104558212A (en) | 2015-04-29 |
| CN104558212B true CN104558212B (en) | 2017-02-22 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111363188B (en) * | 2019-12-17 | 2022-11-11 | 华东理工大学 | Preparation method of ultralight cellulose nanocrystal aerogel material |
| CN113603387B (en) * | 2021-07-15 | 2023-02-10 | 浙江鑫月新材料科技有限公司 | Waterproof concrete synergist and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101973640A (en) * | 2010-09-21 | 2011-02-16 | 东北电力大学 | Method for treating malachite green dye waste water |
| CN102266583A (en) * | 2011-07-10 | 2011-12-07 | 东华大学 | Preparation method of silver-loading modified bacterial cellulose based compound functional wet dressing |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010090591A1 (en) * | 2009-02-05 | 2010-08-12 | Swetree Technologies Ab | Aminated hemicellulose molecule and method for production thereof |
| CN102276736B (en) * | 2011-07-10 | 2013-02-20 | 东华大学 | Selective amination method of bacterial cellulose |
| CN102344496A (en) * | 2011-07-10 | 2012-02-08 | 东华大学 | Method for loading antibacterial nanometer silver by the selectivity of bacteria cellulose |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101973640A (en) * | 2010-09-21 | 2011-02-16 | 东北电力大学 | Method for treating malachite green dye waste water |
| CN102266583A (en) * | 2011-07-10 | 2011-12-07 | 东华大学 | Preparation method of silver-loading modified bacterial cellulose based compound functional wet dressing |
Non-Patent Citations (1)
| Title |
|---|
| 乙二胺螯合细菌纤维素的制备及其吸附Cu2+研究;马波 等;《工业水处理》;20090731;第29卷(第7期);第60-62页，实验方法部分 * |
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