CN109112822A - A method of preparing carbon fiber growth in situ graphene composite carrier - Google Patents
A method of preparing carbon fiber growth in situ graphene composite carrier Download PDFInfo
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- CN109112822A CN109112822A CN201810813941.5A CN201810813941A CN109112822A CN 109112822 A CN109112822 A CN 109112822A CN 201810813941 A CN201810813941 A CN 201810813941A CN 109112822 A CN109112822 A CN 109112822A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/51—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof
- D06M11/55—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with sulfur trioxide; with sulfuric acid or thiosulfuric acid or their salts
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- C12N11/00—Carrier-bound or immobilised enzymes; Carrier-bound or immobilised microbial cells; Preparation thereof
- C12N11/14—Enzymes or microbial cells immobilised on or in an inorganic carrier
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with hydrogen peroxide or peroxides of metals; with persulfuric, permanganic, pernitric, percarbonic acids or their salts
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/68—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
- D06M11/70—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with oxides of phosphorus; with hypophosphorous, phosphorous or phosphoric acids or their salts
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
Abstract
A method of preparing carbon fiber growth in situ graphene composite carrier, the concentrated sulfuric acid is carried out to carbon fiber, phosphoric acid, high price solid chemical compound containing valence variation element, the mixed solution of carbon fiber-containing is obtained after the processing such as hydrogen peroxide, mixed solution is subjected to pickling and washing, solution is simultaneously after concentration washing and the carbon fiber in above-mentioned solution carries out ultrasound together, finally adds reducing agent and is restored to obtain carbon fiber growth in situ graphene composite carrier.The features such as present invention prepares carbon fiber growth in situ graphene composite carrier, has preparation process simple, good surface characteristic and biocompatibility.
Description
Technical field
The present invention relates to carbon material technical field, in particular to a kind of method of carbon fiber growth in situ graphene.
Background technique
For graphene as a kind of emerging carbon family nano material, various features all will predictive of this two-dimension nano materials
Unique fixation support, graphene surface oxygen-containing functional group rich in can be become, and have the effects that pi-pi accumulation power,
Excellent properties can be had shown that in immobilization direction with large biological molecule Non-covalent binding.Graphene has high-ratio surface
Product, the characteristics such as Ultrastrength adhesive and unique carrier make it be used widely in field of biology.Graphene possesses preferably
Biocompatibility, cell proliferation can be promoted.However, at present there is easy to reunite, recyclability in graphene in practical applications
The problems such as poor, thus immobilized cell application in should be modified by the later period, overcome it is easy to reunite, the problems such as being not easily recycled.
Carbon fiber is a kind of high-intensitive, high-modulus new fiber materials, has good biocompatibility, chemical property steady
Surely equal excellent performances, these features determine that carbon fiber has the application potential as good fixation support.But carbon fiber surface
Inertia is big, surface energy is low, and shortage has chemically active functional group, directly affects carbon fibre material answering on immobilization direction
With.Therefore it needs to handle carbon fiber surface, to improve its compatibility and adhesiveness to matrix.
In terms of carbon material carrier, mostly research concentrate on single carbon material as fixation support, be rarely reported about
Graphene and carbon fiber are used for immobilized cell as complex carrier, using carbon fiber as skeleton, carbon fiber growth in situ graphene,
Not only the bigger surface region of graphene can provide the adsorption site of more cells, improve immobilization efficiency, Er Qieyou
In the presence of carbon fiber skeleton, carrier is easy to recycle, and is unfavorable for so as to avoid graphene immobilized cell from reaction
The characteristics of being recycled in liquid.The synergistic effect of its composite material makes carbon fiber while as fixation support skeleton simultaneously,
Also it can play the role of fixation support, weaken immobilization is influenced by single immobilization microenvironment, increases immobilized cell
The stability of related biological property.The patent for being main relevant article below and having disclosed, but it is obviously literary with the application
There is difference in part, such as table 1:
1 part of table discloses the difference of article or patent and application documents
Summary of the invention
It is an object of the invention to prepare carbon fiber growth in situ graphene composite carrier, make carbon fiber surface growth in situ
Graphene, as fixation support immobilized cell.
The technical scheme adopted by the invention is that:
The carbon fiber growth in situ graphene of invention prepares complex carrier, and following methods can be used and be made, comprising the following steps:
In the mixed solution of the concentrated sulfuric acid and phosphoric acid that take suitable carbon fiber to be added to certain volume under the conditions of -5 ~ 20 DEG C,
The high price solid chemical compound containing valence variation element is continuously added under stirring condition, and mixed solution is added after continuing 2 ~ 6h of stirring
40 ~ 60min is reacted in 20 ~ 60 DEG C of water-baths.20 ~ 40 DEG C of deionized water is then added at room temperature, and stir 1 ~ 2h to make its mixing
Uniformly.Then appropriate 30% hydrogen peroxide is added, solution is subjected to pickling and washing, retains solution after washing, is added after concentration
Carbon fiber in above-mentioned solution, 4 ~ 6h of ultrasound adds reducing agent and obtains carbon fiber growth in situ under the conditions of 80 ~ 90 DEG C together
Graphene composite carrier.
Further, in the step of preparation method, the mixed liquor volume that the concentrated sulfuric acid and phosphoric acid is added is carbon fiber:
Mixed liquor volume=(1g:50 ~ 70ml), and the concentrated sulfuric acid and phosphoric acid volume ratio are 10:1.
Further, in the step of preparation method, the high price solid chemical compound of valence variation element is generally potassium permanganate,
Potassium bichromate, chlorate etc..
Further, in the step of preparation method, the volume that hydrogen peroxide is added is carbon fiber: dioxygen water volume=(1g:1
~ 5 ml).
Further, in the step of preparation method, it is carbon fiber: liquor capacity=1g:10 that remaining volume, which is concentrated, in solution
~30 mL。
Beneficial effects of the present invention:
Compared with prior art, it the beneficial effects of the invention are as follows the modifiable characteristic of carbon fiber surface is utilized, omits to carbon fiber
Surface carries out the step of degumming process, is directly surface-treated to carbon fiber surface, increases the hydrophily, coarse on its surface
Degree.The use of phosphoric acid while making growth in situ graphene, increases the biocompatibility of carrier.And the growth of graphene is drawn
Enter oxygen-containing functional group, cell viability can be enhanced, is conducive to immobilization fermentation.
Have preparation process simple using the carbon fiber growth in situ graphene composite carrier that preparation method of the present invention obtains,
The features such as good surface polarity and biocompatibility.The increase of specific surface area can provide more adsorption sites for cell,
The increase of surface polarity further enhances the attraction between carbon fiber surface and cell.The increase of biocompatibility, into one
Step is conducive to the growth and metabolism of immobilized cell.
Using carbon fiber as skeleton, carbon fiber growth in situ graphene, not only fixation support is easy to repeat to recycle,
And single graphene is avoided as fixation support and is unfavorable for the characteristics of recycling in reaction solution.The association of composite material simultaneously
Make carbon fiber while as fixation support skeleton with effect, can also play the role of fixed cell carrier, weakens
Immobilized cell is increased the stability of immobilized cell related biological performance by single immobilization microenvironment.
Detailed description of the invention
Fig. 1 is carbon fiber growth in situ graphene SEM figure.
Fig. 2 is carbon fiber growth in situ graphene XRD diagram.
Fig. 3 be using carbon fiber growth in situ graphene as fixation support immobilized cell fermentation after into the cell
ROS is horizontal.
Specific embodiment
Below with reference to embodiment, specific embodiment of the invention is described in further detail.Following embodiment is to use
The contents of the present invention are further illustrated, without limiting the scope of the invention.For related content according to the present invention
And the modification made, belong to the scope of the present invention.
Embodiment 1:
The preparation of carbon fiber growth in situ graphene composite carrier:
6g carbon fiber is taken to be added in the concentrated sulfuric acid of 300ml and the mixed solution of phosphoric acid (10:1) under the conditions of 10 DEG C, in stirring bar
Potassium hyperchlorate is added under part, and continues that 60min will be reacted in mixed solution 60 DEG C of water-baths of addition after stirring 3h.Then add at room temperature
Enter 25 DEG C of water, and stirring 2h is uniformly mixed it, 30% hydrogen peroxide 20ml is then added.
5% hydrochloric acid of solution and deionized water are washed 3 times respectively, are retained solution after washing, are concentrated into 100mL or so, are added
4 ~ 6h of ultrasound adds 40mL L-AA under the conditions of 80-90 DEG C to chopped carbon fiber in above-mentioned solution together
(40mmol/L) reduction 3h obtains carbon fiber growth in situ graphene composite carrier.
The preparation of carbon fiber growth in situ graphene composite carrier and its application of immobilized cell:
6g carbon fiber is taken to be added in the concentrated sulfuric acid of 300ml and the mixed solution of phosphoric acid (10:1) under the conditions of 10 DEG C, in stirring bar
Potassium bichromate is added under part, and continues that 60min will be reacted in mixed solution 40 DEG C of water-baths of addition after stirring 3h.Then add at room temperature
Enter 25 DEG C of water, and stirring 2h is uniformly mixed it, 30% hydrogen peroxide 10ml is then added.
5% hydrochloric acid of solution and deionized water are washed 3 times respectively, retain solution after washing, retain solution after washing, concentration
To 100 mL or so, ultrasound 4-6h adds 40mL under the conditions of 80-90 DEG C to the chopped carbon fiber being added in above-mentioned solution together
Tea polyphenols (40mmol/L) reduction 3h obtains carbon fiber growth in situ graphene composite carrier.
Carbon fiber growth in situ graphene carrier is used for immobilized cell
Strain: a- hemolytic streptococcus
Seed culture medium: glucose 0.5%, tryptone 0.5%, peptone 0.5%, yeast extract 0.3%, beef extract 0.5%, chlorine
Change sodium 0.5%, pH 7.2
Fermentation medium: peptone 0.3%, yeast extract 0.7%, beef extract 1%, sodium chloride 0.5%, pH 7.2
Immobilization way:
A- hemolytic streptococcus is inoculated into seed culture medium, after culture for 24 hours, by the carbon fiber growth in situ graphene of preparation
Carrier is that 10 g/L are put into aseptic seed culture solution with input amount, is placed in shaking table, control shaking speed is 160
Rpm, shake 0.5~4 h to get.
The application of immobilization:
Progress mannatide is poured out and (poured out 40ml, remaining 10ml) to every batch of after fermentation, by the bacteria suspension in culture medium
Extraction and measurement, and retain complex carrier, add fresh fermentation broth 40ml, mannatide is carried out to fermentation liquid after 48h
It extracts and measures.And so on, carry out multiple batches of fermenting experiment.
The measurement of mannatide in fermentation liquid:
Accurate measuring 20mL fermentation liquid is centrifuged l0min in centrifuge tube at 10000r/min, and removal thallus leaves and takes supernatant；Supernatant
The dehydrated alcohol of 3 times of volumes is added in liquid, 10000r/min after standing is sufficiently stirred, is centrifuged l0min, removal supernatant to obtain the final product
To sediment；By gained sediment l0mL, distilled water dissolution, the trichloroacetic acid tune pH with 15% is 1.5 ~ 3.5, is sufficiently stirred
10000r/min after standing, is centrifuged l0min, and removal impurity obtains supernatant；To going in deimpurity supernatant to be slowly added to
10000r/min, 4 DEG C of centrifugation 10min after standing is sufficiently stirred in the dehydrated alcohol of 40mL.Removal supernatant obtains sediment；
It repeats the above method 2 times, obtained sediment is raw sugar peptide；By gained sediment 1OmL, it is dilute that dissolution is sufficiently stirred in distilled water
It releases.The accurate liquid glucose 0.1mL drawn after different time centrifugation, is diluted to 2mL with sterile water, is compared with sterile water, respectively plus 3%
Phenol solution 1.0mL is added concentrated sulfuric acid 4.5mL, quickly shakes up, and is cooled to after room temperature the progress colorimetric at 490nm, measures light
Density, by regression equation calculation mannosan peptide content.
It is measured in Continuous Fermentation Processes in the present embodiment, the fixation cell of carbon fiber growth in situ graphene fixation support
Born of the same parents' efficiency is 35~50%, and its immobilized cell can be used continuously 6 ~ 8 times, and fermentation yield is 1g/L or so, relative to free thin
Born of the same parents improve 40%.
Claims (3)
1. a kind of prepare carbon fiber growth in situ graphene composite carrier, which is characterized in that following methods can be used and be made:
It takes suitable carbon fiber to be added in the concentrated sulfuric acid of certain volume and the mixed solution of phosphoric acid under the conditions of -5 ~ 20 DEG C, is stirring
The high price solid chemical compound containing valence variation element is continuously added under the conditions of mixing, and continues that mixed solution is added 20 after 2 ~ 6h of stirring
40 ~ 60min is reacted in ~ 60 DEG C of water-bath；20 ~ 40 DEG C of deionized water is then added at room temperature, 1 ~ 2h of stirring makes its mixing
Uniformly；Then appropriate 30% hydrogen peroxide is added, and solution is subjected to pickling and washing, retains solution after washing, is added after concentration
Carbon fiber in above-mentioned solution, 4 ~ 6h of ultrasound, adds weak reductant at 80 ~ 90 DEG C and obtains carbon fiber growth in situ graphite together
Alkene complex carrier.
2. it is characterized in that, the volume ratio of the concentrated sulfuric acid and phosphoric acid is 10 ~ 20 in preparation method according to claim 1:
1。
3. it is characterized in that, aqueous solution need to pass through concentration in preparation method according to claim 1, and being remained after being concentrated
Remaining volume is carbon fiber: liquor capacity=1g:10 ~ 30 mL.
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