CN107006518A - A kind of preparation method of the plain composite of antibiotic carbon fiber - Google Patents
A kind of preparation method of the plain composite of antibiotic carbon fiber Download PDFInfo
- Publication number
- CN107006518A CN107006518A CN201710281061.3A CN201710281061A CN107006518A CN 107006518 A CN107006518 A CN 107006518A CN 201710281061 A CN201710281061 A CN 201710281061A CN 107006518 A CN107006518 A CN 107006518A
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- China
- Prior art keywords
- copper
- bacteria cellulose
- preparation
- carbon fiber
- dried
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Classifications
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
- A01N59/20—Copper
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
Abstract
The invention discloses a kind of preparation method of the plain composite of antibiotic carbon fiber; by the way that the bacteria cellulose after freeze-drying is immersed in copper salt solution; carry out carbonization treatment after drying under inert atmosphere protection again, finally obtain the carbon fibre composite with good anti-microbial property and bio-compatible performance.Preparation process of the present invention is simple, and easy to operate, cost is low, copper particle is smaller in composite and is dispersed in the three-dimensional grid of carbonization bacteria cellulose, the copper particle that is fettered by grid is difficult to come off from carbon fiber simultaneously, and through flowing water continuous flushing 5 hours, copper turnover rate was only 1.52%.Copper-loaded carbonization bacteria cellulose durable antibacterial effect prepared by the present invention is stable, can preserve for a long time, available for common antiseptic dressing, it may also be used for the field such as water process.
Description
Technical field
The invention belongs to the preparing technical field of antiseptic, and in particular to a kind of preparation of the plain composite of antibiotic carbon fiber
Method.
Background technology
Activated carbon fiber has huge ratio surface and abundant micropore, and adsorption/desorption speed is fast, it is easy to be processed into all kinds of
The characteristics of character, just progressively replace traditional sorbing material activated carbon, in gas absorption purification, the neck such as sewage disposal, purifying of drinking water
Domain is applied.
Metallic copper has had thousands of years of history as a kind of antiseptic, is just stored up early in the India before more than 4000 years with Copper Pot
Water sterilization.Copper is the indispensable micronutrient of health, for blood, nervous centralis and immune system, hair, skin
Development and function with the internal organ such as skeletal tissue and brain and liver, the heart have a major impact.Compared with silver, copper is not only cheap,
And with higher chemical stability and environmental safety.
Bacteria cellulose is to be metabolized a kind of cellulose base large biological molecule synthesized by acetobacter xylinum.Compared to string
Element, it has great advantage in terms of purity, the degree of polymerization, crystallinity and orientation.Bacteria cellulose aquagel is chilled dry
The processing of dry or supercritical drying obtains bacteria cellulose aeroge, further across high temperature cabonization processing, obtains carbonization bacterium fine
Dimension element.The bacteria cellulose that is carbonized has unique tridimensional network, high porosity, the fiber size of nanoscale and good
Good structural stability, the different element by mixing can obtain the composite of excellent performance.Chinese patent
To be carbonized bacteria cellulose and magnetic materials of CN102093840A is combined, and obtains network carbon nanofiber element/magnetic coupling
Material, can be used as preferable microwave absorption.Chinese patent CN105053007A, compound receive is prepared using the method for in-situ reducing
Meter Yin bacteria cellulose, is answered through in sterile heat-treatment furnace, obtaining the nanometer carbon aerogels antibacterial with good anti-microbial property
Condensation material, but the cost of silver is high, and Ag+Easily with the Cl in aqueous medium-、HS-、S2-And SO4 2-Etc. reacting, formed water insoluble
Precipitation, so as to lose antibacterial activity.
The content of the invention
It is an object of the invention to provide a kind of preparation method of the plain composite of antibiotic carbon fiber, use bacteria cellulose for
Raw material, by easy copper salt solution immersion process, then through carbonization treatment, nano copper particle is loaded on carbon fiber, obtained
The carbon fibre material containing nano copper particle with good anti-microbial property.
Technical scheme is as follows：
A kind of preparation method of the plain composite of antibiotic carbon fiber, using bacteria cellulose as raw material, soaking normal direction bacterium
Copper ion is introduced in cellulose, copper-loaded carbonization bacteria cellulose is prepared by high temperature cabonization, comprised the following steps that：
Step 1, bacteria cellulose is freeze-dried；
Step 2, pretreated bacteria cellulose is immersed in copper salt solution, takes out and be dried to obtain cupric after cleaning
Composite bacterial cellulose；
Step 3, under inert atmosphere protection, with 1-10 DEG C/min programming rate, 600-1400 DEG C is warming up to, by cupric
Composite bacterial cellulose carries out carbonization treatment, is incubated 6-20h, copper-loaded carbonization bacteria cellulose, i.e. antibacterial carbon is obtained after cooling fine
The plain composite of dimension.
In step 1, the time of described freeze-drying is 12~48h.
In step 2, described mantoquita is copper chloride, copper sulphate or copper nitrate, described mantoquita and the matter of bacteria cellulose
Amount is than being 0.01~0.1：1, soak time is 0.5~48h, and soaking temperature is 10~90 DEG C, and washing times are 1~5 time, are dried
To be dried in vacuo or being freeze-dried.
In step 3, described inert gas is nitrogen or argon gas.
Preparation is simple, easy to operate, cost is low by the present invention, utilizes the carbon of bacteria cellulose vacuum pyrolysis formation
As reducing agent, copper-loaded and carbonization is completed in a step, atom economy is realized, while simplifying the preparation of material
Journey.The copper-loaded carbonization bacteria cellulose that the present invention is obtained has good spacial framework, and copper particle is smaller and can uniformly divide
In the three-dimensional grid for being dispersed in carbonization bacteria cellulose, while the copper particle fettered by grid is also not easy to come off from carbon fiber,
Through flowing water continuous flushing 5 hours, copper turnover rate was only 1.52%.Copper-loaded carbonization bacteria cellulose antibacterial effect prepared by the present invention
Lasting stability, can be preserved for a long time.
Brief description of the drawings
Fig. 1 is the transmission electron microscope picture of the plain composite of antibiotic carbon fiber prepared by embodiment 1.
Embodiment
The present invention is described in further detail with reference to embodiment and accompanying drawing.
Embodiment 1
Step 1, bacteria cellulose is placed in into freeze drier to be freeze-dried 12 hours；
Step 2, that the bacteria cellulose that 1g is dried is immersed in the solution containing 0.01g copper nitrates into 10 DEG C of immersions 0.5 is small
When, take out and be dried in vacuo after washing 1 time；
Step 3, the cupric composite bacterial cellulose that step 2 is obtained is put into heating furnace under nitrogen atmosphere protection with 1
DEG C/min firing rates are heated to 600 DEG C, 6 hours are incubated, room temperature is then cooled to 1 DEG C/min cooling velocities, obtains copper-loaded
Be carbonized bacteria cellulose.
Fig. 1 is the transmission electron microscope picture of copper-loaded carbonization bacteria cellulose prepared by embodiment 1.Nano-grade size as seen from the figure
Copper particle is relatively uniformly dispersed throughout in the three-dimensional grid of carbonization bacteria cellulose, and copper particle is smaller and distribution uniform, average grain
Footpath 76nm.
Embodiment 2
Step 1, bacteria cellulose is placed in into freeze drier to be freeze-dried 24 hours；
Step 2, that the bacteria cellulose that 1g is dried is immersed in the solution containing 0.05g copper sulphate into 20 DEG C of immersions 0.5 is small
When, take out and be dried in vacuo after washing 2 times；
Step 3, the cupric composite bacterial cellulose that step 2 is obtained is put into heating furnace under argon gas atmosphere protection with 2
DEG C/min firing rates are heated to 800 DEG C, 8 hours are incubated, room temperature is then cooled to 1 DEG C/min cooling velocities, obtains copper-loaded
Be carbonized bacteria cellulose.
Embodiment 3
Step 1, bacteria cellulose is placed in into freeze drier to be freeze-dried 48 hours；
Step 2, the bacteria cellulose that 1g is dried is immersed in the solution containing 0.1g copper sulphate into 90 DEG C to soak 48 hours,
Take out and be freeze-dried after washing 5 times；
Step 3, the cupric composite bacterial cellulose that step 2 is obtained is put into heating furnace under argon gas atmosphere protection with 5
DEG C/min firing rates are heated to 1400 DEG C, 20 hours are incubated, room temperature is then cooled to 5 DEG C/min cooling velocities, carried
Copper carbonization bacteria cellulose.
Embodiment 4
Step 1, bacteria cellulose is placed in into freeze drier to be freeze-dried 48 hours；
Step 2, the bacteria cellulose that 1g is dried is immersed in the solution containing 0.1g copper nitrates into 90 DEG C to soak 48 hours,
Take out and be freeze-dried after washing 3 times；
Step 3, the cupric composite bacterial cellulose that step 2 is obtained is put into heating furnace under argon gas atmosphere protection with 5
DEG C/min firing rates are heated to 1400 DEG C, 20 hours are incubated, room temperature is then cooled to 5 DEG C/min cooling velocities, carried
Copper carbonization bacteria cellulose.
Embodiment 5
Step 1, bacteria cellulose is placed in into freeze drier to be freeze-dried 36 hours；
Step 2, that the bacteria cellulose that 1g is dried is immersed in the solution containing 0.02g copper nitrates into 70 DEG C of immersions 36 is small
When, take out and be freeze-dried after washing 2 times；
Step 3, the cupric composite bacterial cellulose that step 2 is obtained is put into heating furnace under argon gas atmosphere protection with 6
DEG C/min firing rates are heated to 1200 DEG C, 10 hours are incubated, room temperature is then cooled to 5 DEG C/min cooling velocities, carried
Copper carbonization bacteria cellulose.
Embodiment 6
Step 1, bacteria cellulose is placed in into freeze drier to be freeze-dried 40 hours；
Step 2, that the bacteria cellulose that 1g is dried is immersed in the solution containing 0.02g copper sulphate into 40 DEG C of immersions 30 is small
When, take out and be freeze-dried after washing 3 times；
Step 3, the cupric composite bacterial cellulose that step 2 is obtained is put into heating furnace under nitrogen atmosphere protection with 10
DEG C/min firing rates are heated to 1000 DEG C, 9 hours are incubated, room temperature is then cooled to 10 DEG C/min cooling velocities, carried
Copper carbonization bacteria cellulose.
The sterilizing rate (%) of the copper-loaded carbonization bacteria cellulose of table 1
Copper-loaded carbonization bacteria cellulose made from embodiment 1~6 is subjected to anti-microbial property test, testing procedure is as follows：
In the triangular flask for filling 20mL test organisms, the copper-loaded carbonization bacteria celluloses of 2mg are added, test organisms initial concentration is 107cfu/mL.
Shaken cultivation 24 hours in 37 DEG C of shaking tables, then residual viable bacteria bacterial concentration in triangular flask is determined with dilution-plate method, to test load
The antibiotic and sterilizing performance of copper carbonization bacteria cellulose.Each antibacterial tests carry out blank control test simultaneously.As a result such as the institute of table 1
Show.As can be seen from the table, the copper-loaded carbonization bacteria cellulose that prepared by embodiment 1~6 is to Escherichia coli and Staphylococcus aureus
Bacterium has strong antibiotic and sterilizing ability.
Claims (4)
1. the preparation method of the plain composite of a kind of antibiotic carbon fiber, it is characterised in that comprise the following steps that：
Step 1, bacteria cellulose is freeze-dried；
Step 2, pretreated bacteria cellulose is immersed in copper salt solution, takes out and the compound of cupric is dried to obtain after cleaning
Bacteria cellulose；
Step 3, under inert atmosphere protection, with 1-10 DEG C/min programming rate, 600-1400 DEG C is warming up to, by the compound of cupric
Bacteria cellulose carries out carbonization treatment, is incubated 6-20h, and copper-loaded carbonization bacteria cellulose, i.e. antibiotic carbon fiber element are obtained after cooling
Composite.
2. preparation method according to claim 1, it is characterised in that in step 1, the time of described freeze-drying is 12
~48h.
3. preparation method according to claim 1, it is characterised in that in step 2, described mantoquita is copper chloride, sulfuric acid
Copper or copper nitrate, described mantoquita and the mass ratio of bacteria cellulose are 0.01~0.1：1, soak time is 0.5~48h, leaching
It is 10~90 DEG C to steep temperature, and washing times are 1~5 time, dries as vacuum drying or is freeze-dried.
4. preparation method according to claim 1, it is characterised in that in step 3, described inert gas is nitrogen or argon
Gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710281061.3A CN107006518A (en) | 2017-04-26 | 2017-04-26 | A kind of preparation method of the plain composite of antibiotic carbon fiber |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710281061.3A CN107006518A (en) | 2017-04-26 | 2017-04-26 | A kind of preparation method of the plain composite of antibiotic carbon fiber |
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| Publication Number | Publication Date |
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| CN107006518A true CN107006518A (en) | 2017-08-04 |
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| CN201710281061.3A Pending CN107006518A (en) | 2017-04-26 | 2017-04-26 | A kind of preparation method of the plain composite of antibiotic carbon fiber |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110100821A (en) * | 2019-04-29 | 2019-08-09 | 山东省农业科学院植物保护研究所 | A kind of biological agent and the preparation method and application thereof for preventing and treating the late blight of potato |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105053007A (en) * | 2015-08-06 | 2015-11-18 | 北京科技大学 | Preparation method of novel high performance antibacterial nano-cellulose carbon aerogel |
| CN105311668A (en) * | 2015-10-30 | 2016-02-10 | 东华大学 | Bacterial cellulose compound cuprous oxide antimicrobial dressing and preparation method thereof |
| CN105521783A (en) * | 2016-01-05 | 2016-04-27 | 北京林业大学 | Biomass carbon base and copper and/or cuprous oxide hybrid material, and preparation method thereof |
| CN105641734A (en) * | 2016-02-23 | 2016-06-08 | 南京荣之盛生物科技有限公司 | Preparation method of slow-release type bacterial cellulose based antibacterial agent |
| CN106512876A (en) * | 2016-11-17 | 2017-03-22 | 陕西盛迈石油有限公司 | Preparation method of carbonized bacterial cellulose wrapped copper |
-
2017
- 2017-04-26 CN CN201710281061.3A patent/CN107006518A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105053007A (en) * | 2015-08-06 | 2015-11-18 | 北京科技大学 | Preparation method of novel high performance antibacterial nano-cellulose carbon aerogel |
| CN105311668A (en) * | 2015-10-30 | 2016-02-10 | 东华大学 | Bacterial cellulose compound cuprous oxide antimicrobial dressing and preparation method thereof |
| CN105521783A (en) * | 2016-01-05 | 2016-04-27 | 北京林业大学 | Biomass carbon base and copper and/or cuprous oxide hybrid material, and preparation method thereof |
| CN105641734A (en) * | 2016-02-23 | 2016-06-08 | 南京荣之盛生物科技有限公司 | Preparation method of slow-release type bacterial cellulose based antibacterial agent |
| CN106512876A (en) * | 2016-11-17 | 2017-03-22 | 陕西盛迈石油有限公司 | Preparation method of carbonized bacterial cellulose wrapped copper |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110100821A (en) * | 2019-04-29 | 2019-08-09 | 山东省农业科学院植物保护研究所 | A kind of biological agent and the preparation method and application thereof for preventing and treating the late blight of potato |
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Application publication date: 20170804 |
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