CN109369972A - Tuna collagen-chitosan complex film frequency sweep ultrasonic preparation method - Google Patents
Tuna collagen-chitosan complex film frequency sweep ultrasonic preparation method Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D65/00—Wrappers or flexible covers; Packaging materials of special type or form
- B65D65/38—Packaging materials of special type or form
- B65D65/46—Applications of disintegrable, dissolvable or edible materials
- B65D65/463—Edible packaging materials
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/246—Intercrosslinking of at least two polymers
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Abstract
The invention discloses tuna collagen-chitosan complex film frequency sweep ultrasonic preparation methods, belong to packaging material for food preparation technical field.It is extracted from tuna skin first with pepsin and obtains pepsin-solubilized collagen；Then tuna collagen-chitosan edible composite film is prepared using frequency sweep ultrasonic auxiliary.Using tuna collagen-chitosan edible composite film of frequency sweep ultrasonic technology auxiliary preparation, compared to the composite membrane without ultrasound, the mechanical performance of film is more preferable, and tensile strength and elongation at break are significantly increased.The biocompatibility of the film is good, and degradable and fresh-keeping function is preferable, and primary raw material and auxiliary material are Edible material, safe and non-toxic, environmentally protective, and source is sufficient and cost is relatively low.The present invention develops new edible membrane material for China's food packaging industry and provides certain technical parameter and theoretical direction.
Description
Technical field
The present invention relates to packaging material for food preparation technical fields, refer in particular to one kind with tuna collagen and chitosan
For raw material, the method for preparing edible film using frequency sweep ultrasonic processing.
Background technique
In recent years, people are higher and higher to environmental protection and food safety requirements, also proposed more to packaging material for food
High requirement, degradable and Nantural non-toxic edible film are increasingly becoming the research hotspot of food packaging applications.
Tuna contains abundant protein, and protein bio potency is a kind of ammonia compared to high compared with meat and other fish
Base acid forms excellent protein, has very high nutritive value and economic value.Tuna skin is tuna processing
Main By product, collagen content is still very high, but is not fully utilized, as feed or is directly discarded, economical
It is worth low and pollution environment.Therefore, fish-skin resource how is made full use of, is turned waste into wealth, is reduced environmental pollution, is domestic and international at present
The project that researcher increasingly pays close attention to.
Edible film is that a kind of substance (such as protein and polysaccharide) with edible natural is film forming matrix, passes through difference
Intermolecular interaction and formed can obstruct moisture, fragrance scatters and disappears and dioxygen oxidation etc. and with certain mechanical performance
Film.Collagen is due to its low antigenicity, biodegradability, good mechanical property and biocompatibility, it is considered to be
One of the most useful natural polymer biomaterial.Chitosan is a kind of linear polymeric material of edibility, nontoxic, can drop
Solution, good biocompatibility have good film forming, are the raw materials of very promising manufacture edible film.Due to collagen
Good compatibility is all had with chitosan, the two is learnt from other's strong points to offset one's weaknesses, and mechanical and antibacterial good properties can be made by synergistic effect
Biological composite membrane.
Currently, conventional compound membrane preparation method is usually to configure certain density collagen and chitosan solution, press
Certain proportion mixing, is added suitable glycerol and makees plasticizer, and a period of time of grafting at a certain temperature, then re-dry prepared tool
There are certain mechanical strength, the film of compact structure.But the mechanical performance of the composite membrane of conventional method preparation at present is not still high.
To solve the above-mentioned problems, at present studies have reported that promoting albumen to achieve certain with the graft reaction of sugar using ultrasonic wave
The functional characteristic of effect, product is improved.But it is typically all to use single-frequency that ultrasound, which promotes albumen-sugar Study on graft reaction, at present
Ultrasound, mechanical performance improvement effect be not significant.However, not having also from the point of view of according to the document report studied at present by pulse, frequency sweep etc.
Advanced ultrasound mode is used for tuna collagen-chitosan edible film preparation research.
Summary of the invention
To solve the above problems, the present invention introduces in tuna collagen-chitosan complex film preparation process
Advanced frequency sweep ultrasonic technology can give full play to the synergistic effect of impulse ultrasound and frequency sweep ultrasonic, promote collagen and shell
The crosslinking of glycan obtains a kind of edible composite membrane that structure is more compact, significantly improves the mechanical performance of composite membrane.
The frequency sweep ultrasonic preparation method of tuna collagen-chitosan complex film of the present invention, according to following
Step carries out:
(1) tuna collagen is prepared: by the fish-skin after degreasing removing impurities albumen, with solid-liquid ratio 1:70 (mg/mL) leaching
It steeps in 0.5M acetic acid solution, the pepsin (pH=2) of 0.06% (W/V) 1800U/g of addition, the homogeneous 5min in ice bath, 4
DEG C enzymolysis and extraction 48h is centrifuged 45min in 4 DEG C of 10000r/min, and supernatant is collagen crude extract.Collagen slightly mentions
Liquid adds NaCl to 0.9M to saltout overnight, and 6000r/min is centrifuged 20min, and gained precipitating is dissolved in 0.5M acetic acid, 10000r/min
It is centrifuged 45min, gained supernatant adds NaCl to 2.4M to saltout overnight, and 6000r/min is centrifuged 20min, and gained precipitating is dissolved in
In 0.5M acetic acid, dialyses three days, obtain collagen through vacuum freeze drying.
(2) tuna collagen-chitosan mixed liquor: the collagen that the step of weighing certain mass (1) obtains is prepared
Albumen is configured to the collagen solution of 2g/100mL with distilled water in beaker, and 30min is dissolved in 50 DEG C of water-baths, and suction filtration obtains
Pure collagen solution.The chitosan of certain mass is weighed in beaker, the glacial acetic acid that 2% (V/V) is added is made into 2g/
The chitosan solution of 100mL, 50 DEG C of water-baths are dissolved 30min, are stood overnight.By collagen and chitosan solution according to mass ratio
1:4 mixing, and 25% (accounting for total soluble matters mass ratio) glycerol is added and makees plasticizer, stirring 10min is uniformly mixed so as to obtain mixed under the conditions of 20 DEG C
Close liquid.
(3) mixed liquor in step (2) is subjected to frequency sweep ultrasonic processing, obtains ULTRASONIC COMPLEX film liquid.It is ultrasonically treated parameter
Are as follows: frequency 28kHz；Power density 100W/L；20~500ms of frequency sweep cycle；Frequency sweep amplitude 0~± 2.0kHz；Pulse duty factor
20%~90%；Total time 10min.After ultrasonic treatment, mixed liquor is crosslinked 50min in 55 DEG C of water-bath.
(4) composite membrane liquid that step (3) obtains is laid in clean polyethylene ware respectively, is dried under the conditions of 40 DEG C
24h.It is taken out after drying, takes off film with blade after film is cooled to room temperature and obtain tuna collagen-chitosan complex film.
Wherein molecular weight of chitosan described in step (2) is 100,000 dalton.
Wherein frequency sweep ultrasonic frequency sweep cycle described in step (3) are as follows: 20,100,200,300,500, preferably 100ms.
Wherein frequency sweep ultrasonic frequency sweep amplitude described in step (3) are as follows: 0, ± 0.5, ± 1.0, ± 1.5, ± 2.0, preferably
For ± 0.5kHz.
Wherein frequency sweep ultrasonic pulse duty factor described in step (3) are as follows: 20% (10s/40s), 50% (10s/10s),
70% (10s/3s), 90% (24s/3s), preferably 77%.
The beneficial effects of the present invention are:
(1) the raw material tuna skin that the present invention chooses is the waste after tuna processing, is mainly used as feed or straight
It connects and is dropped, the utilization rate of tuna skin is very low, causes the serious waste of tuna skin resource；The present invention is separated using it as raw material
Collagen is extracted, tuna collagen-chitosan edible film is prepared, is conducive to the synthesis of tuna processing byproduct
It utilizes, while improving the added value of tuna skin.
(2) it is super to introduce advanced frequency sweep in tuna collagen-chitosan complex film preparation process by the present invention
Audio technology gives full play to the synergistic effect of impulse ultrasound and frequency sweep ultrasonic, promotes the crosslinking of collagen and chitosan, obtains one
The more compact edible composite membrane of kind structure, compared with not sonicated composite membrane, the mechanical performance of composite membrane is significant
It improves.
(3) tuna of the invention collagen-chitosan complex film frequency sweep ultrasonic preparation method, technological operation letter
Single, all raw materials are safe and non-toxic, and organic reagent is not directed in preparation process, are suitble to industrialized production.Widen edible film
Research direction, it is intended to develop new edible membrane material for China's food packaging industry certain technical parameter and theory are provided and refer to
It leads.
Detailed description of the invention
Fig. 1 is frequency sweep ultrasonic equipment structure chart.
The reference numerals are as follows:
1 is electrically heated rod, and 2 be temp probe, and 3 be ultrasonic pond, and 4 be ultrasonic transducer (vibration plate under ultrasonic wave), and 5 is out
Liquid mouth (band valve), 6 be computer controller, and 7 be ultrasonic wave controller.
Specific embodiment:
The present invention is described in further detail below with reference to specific embodiment, and referring to data.Illustrate hereby, these realities
It is of the invention solely for the purpose of illustration to apply example, rather than limits the scope of the invention in any way.
Fig. 1 is the frequency sweep ultrasonic processing equipment that the present invention uses, and is Jiangsu University's independent development.The equipment is furnished with an electricity
Brain cyclelog 6, can set ultrasound works parameter (frequency, power density, frequency sweep cycle, frequency sweep amplitude, pulse duty factor,
Total time), ultrasonic wave controller 7 is controlled, being connected to frequency is the ultrasonic transducer 4 of 28kHz, it can be achieved that at frequency sweep ultrasonic wave
Reason；Compound coating solution is placed in sample sack and is put into ultrasonic pond 3, different ultrasonic treatment tests are carried out.Pass through 1 He of electrically heated rod
The control of the realization ultrasonic temperature of temp probe 2.
Chitosan in the present invention is commercial product, and molecular weight is 100,000 dalton.
Tuna collagen in the present invention is prepared in the steps below:
It by the fish-skin after degreasing removing impurities albumen, is soaked in 0.5M acetic acid solution, is added with solid-liquid ratio 1:70 (mg/mL)
The pepsin (pH=2) of 0.06% (W/V) 1800U/g, the homogeneous 5min in ice bath, 4 DEG C of enzymolysis and extraction 48h, in 4 DEG C
10000r/min is centrifuged 45min, and supernatant is collagen crude extract.Collagen crude extract adds NaCl to 0.9M to saltout
Night, 6000r/min are centrifuged 20min, and gained precipitating is dissolved in 0.5M acetic acid, and 10000r/min is centrifuged 45min, gained supernatant
NaCl to 2.4M is added to saltout overnight, 6000r/min is centrifuged 20min, and gained precipitating is dissolved in 0.5M acetic acid, dialyses three days, warp
Vacuum freeze drying obtains collagen.Collagen recovery rate is 70% after measured, purity 90%.
Embodiment 1:
Not sonicated tuna collagen-chitosan complex film preparation method, as steps described below into
Row:
(1) collagen of certain mass is weighed in beaker, and the collagen for being configured to 2g/100mL with distilled water is molten
30min is dissolved in liquid, 50 DEG C of water-baths, and suction filtration obtains pure collagen solution.The chitosan of certain mass is weighed in beaker,
The glacial acetic acid that 2% (V/V) is added is made into the chitosan solution of 2g/100mL, and 50 DEG C of water-baths are dissolved 30min, stood overnight.By glue
Former albumen is mixed with chitosan solution according to mass ratio 1:4, and 25% (accounting for total soluble matters mass ratio) glycerol is added and makees plasticizer, and 20
10min is stirred under the conditions of DEG C is uniformly mixed so as to obtain mixed liquor.
(2) mixed liquor in step (1) is crosslinked in 55 DEG C of water-bath to 1h and obtains non-ULTRASONIC COMPLEX film liquid.
(3) the non-ULTRASONIC COMPLEX film liquid for obtaining step (2) is laid in clean polyethylene ware, is dried under the conditions of 40 DEG C
24h.It is taken out after drying, takes off film with blade after film is cooled to room temperature and obtain tuna collagen-chitosan complex film.
It saves it in (25 ± 0.5) DEG C, dry in the drier of relative humidity 58% or so equipped with being adjusted with saturation sodium bromide solution
2d measures the mechanical performance of composite membrane.
(4) Measuring Mechanical Properties of composite membrane:
The measurement of tensile strength (TS) and elongation at break (EAB): the smooth unabroken film of selection is simultaneously cut into 20mm
The strip of × 60mm measures its tensile strength and elongation at break with physical property instrument.Rate of extension is 60mm/min, and gauge length is
40mm。
Tensile strength calculation formula: TS=F/ (d × W)
In formula: TS-tensile strength (MPa)；The maximum tension (N) born when F-film fracture；D-film thickness (mm)；W—
Film width (mm).
Elongation at break calculation formula: EAB=(L-L0)×100/L0
In formula: EAB-elongation at break (%)；The distance between graticule (mm) when L-film fracture；L0The original graticule of-film
Distance (mm).
The concrete outcome of tensile strength and elongation at break is shown in Table 1.
Embodiment 2:
Tuna collagen-chitosan complex film preparation method of different frequency sweep cycle processing, according to following steps
It is rapid to carry out:
(1) collagen of certain mass is weighed in beaker, and the collagen for being configured to 2g/100mL with distilled water is molten
30min is dissolved in liquid, 50 DEG C of water-baths, and suction filtration obtains pure collagen solution.The chitosan of certain mass is weighed in beaker,
The glacial acetic acid that 2% (V/V) is added is made into the chitosan solution of 2g/100mL, and 50 DEG C of water-baths are dissolved 30min, stood overnight.By glue
Former albumen is mixed with chitosan solution according to mass ratio 1:4, and 25% (accounting for total soluble matters mass ratio) glycerol is added and makees plasticizer, and 20
10min is stirred under the conditions of DEG C is uniformly mixed so as to obtain mixed liquor.
(2) mixed liquor in step (1) is ultrasonically treated parameter are as follows: frequency in 55 DEG C of progress frequency sweep ultrasonic processing
28kHz；Power density 100W/L；Frequency sweep cycle 20ms；Frequency sweep amplitude ± 1.0kHz；Pulse duty factor 77% (10s/3s)；Always
Time 10min.After ultrasonic treatment, mixed liquor is crosslinked 50min in 55 DEG C of water-bath.
(3) the ULTRASONIC COMPLEX film liquid that step (2) obtains is laid in clean polyethylene ware, is dried under the conditions of 40 DEG C
24h.It is taken out after drying, takes off film with blade after film is cooled to room temperature and obtain tuna collagen-chitosan complex film.
It saves it in (25 ± 0.5) DEG C, dry in the drier of relative humidity 58% or so equipped with being adjusted with saturation sodium bromide solution
2d measures the mechanical performance of composite membrane.
(4) Measuring Mechanical Properties of composite membrane:
The measurement of tensile strength (TS) and elongation at break (EAB): the smooth unabroken film of selection is simultaneously cut into 20mm
The strip of × 60mm measures its tensile strength and elongation at break with physical property instrument.Rate of extension is 60mm/min, and gauge length is
40mm。
Tensile strength calculation formula: TS=F/ (d × W)
In formula: TS-tensile strength (MPa)；The maximum tension (N) born when F-film fracture；D-film thickness (mm)；W—
Film width (mm).
Elongation at break calculation formula: EAB=(L-L0)×100/L0
In formula: EAB-elongation at break (%)；The distance between graticule (mm) when L-film fracture；L0The original graticule of-film
Distance (mm).
The concrete outcome of tensile strength and elongation at break is shown in Table 1.
Embodiment 3:
The frequency sweep cycle of ultrasonic treatment is 100ms, remaining step is the same as embodiment 2；The tool of tensile strength and elongation at break
Body the results are shown in Table 1.
Embodiment 4:
The frequency sweep cycle of ultrasonic treatment is 200ms, remaining step is the same as embodiment 2；The tool of tensile strength and elongation at break
Body the results are shown in Table 1.
Embodiment 5:
The frequency sweep cycle of ultrasonic treatment is 300ms, remaining step is the same as embodiment 2；The tool of tensile strength and elongation at break
Body the results are shown in Table 1.
Embodiment 6:
The frequency sweep cycle of ultrasonic treatment is 500ms, remaining step is the same as embodiment 2；The tool of tensile strength and elongation at break
Body the results are shown in Table 1.
Influence of the different frequency sweep cycles of table 1 to composite membrane tensile strength and elongation at break
| Embodiment | Frequency sweep cycle ms | Tensile strength MPa | Elongation at break % |
| Comparative example (i.e. embodiment 1) | Ultrasound is not added | 15.2 | 51.9 |
| Embodiment 2 | 20 | 15.7 | 50.0 |
| Embodiment 3 | 100 | 17.8 | 55.9 |
| Embodiment 4 | 200 | 18.3 | 53.0 |
| Embodiment 5 | 300 | 15.4 | 50.0 |
| Embodiment 6 | 500 | 16.1 | 47.1 |
By composite membrane tensile strength and the elongation at break of comparative example 1 in table 1 and embodiment 2-6 it can be found that
(ultrasound is not added) compared with the control, the ultrasonic treatment of different frequency sweep cycles can make the tensile strength of composite membrane improve 1.3%-
The ultrasonic treatment of 20.4%, especially frequency sweep cycle 100ms and 200ms make the tensile strength of composite membrane improve 17.1% respectively
With 20.4%.Frequency sweep cycle 100ms's and 200ms is ultrasonically treated while also improving the elongation at break of composite membrane, frequency sweep week
The ultrasonic treatment of phase 100ms influences maximum to the elongation at break of composite membrane, improves 7.7%.It is obtained by the above results, from again
From the point of view of the tensile strength and the elongation at break that close film, certain frequency sweep ultrasonic processing keeps the mechanical performance of composite membrane more preferable,
When middle frequency sweep cycle is 100ms, the mechanical performance for obtaining composite membrane is optimal.
Embodiment 7:
Tuna collagen-chitosan complex film preparation method of different frequency sweep the amplitude processings, according to following steps
It is rapid to carry out:
(1) collagen of certain mass is weighed in beaker, and the collagen for being configured to 2g/100mL with distilled water is molten
30min is dissolved in liquid, 50 DEG C of water-baths, and suction filtration obtains pure collagen solution.The chitosan of certain mass is weighed in beaker,
The glacial acetic acid that 2% (V/V) is added is made into the chitosan solution of 2g/100mL, and 50 DEG C of water-baths are dissolved 30min, stood overnight.By glue
Former albumen is mixed with chitosan solution according to mass ratio 1:4, and 25% (accounting for total soluble matters mass ratio) glycerol is added and makees plasticizer, and 20
10min is stirred under the conditions of DEG C is uniformly mixed so as to obtain mixed liquor.
(2) mixed liquor in step (1) is ultrasonically treated parameter are as follows: frequency in 55 DEG C of progress frequency sweep ultrasonic processing
28kHz；Power density 100W/L；Frequency sweep cycle 100ms；Frequency sweep amplitude 0kHz；Pulse duty factor 77% (10s/3s)；Total time
10min.After ultrasonic treatment, mixed liquor is crosslinked 50min in 55 DEG C of water-bath.
(3) the ULTRASONIC COMPLEX film liquid that step (2) obtains is laid in clean polyethylene ware, is dried under the conditions of 40 DEG C
24h.It is taken out after drying, takes off film with blade after film is cooled to room temperature and obtain tuna collagen-chitosan complex film.
It saves it in (25 ± 0.5) DEG C, dry in the drier of relative humidity 58% or so equipped with being adjusted with saturation sodium bromide solution
2d measures the mechanical performance of composite membrane.
(4) Measuring Mechanical Properties of composite membrane:
The measurement of tensile strength (TS) and elongation at break (EAB): the smooth unabroken film of selection is simultaneously cut into 20mm
The strip of × 60mm measures its tensile strength and elongation at break with physical property instrument.Rate of extension is 60mm/min, and gauge length is
40mm。
Tensile strength calculation formula: TS=F/ (d × W)
In formula: TS-tensile strength (MPa)；The maximum tension (N) born when F-film fracture；D-film thickness (mm)；W—
Film width (mm).
Elongation at break calculation formula: EAB=(L-L0)×100/L0
In formula: EAB-elongation at break (%)；The distance between graticule (mm) when L-film fracture；L0The original graticule of-film
Distance (mm).
The concrete outcome of tensile strength and elongation at break is shown in Table 2.
Embodiment 8:
The frequency sweep amplitude of ultrasonic treatment is ± 0.5kHz, remaining step is the same as embodiment 7；Tensile strength and elongation at break
Concrete outcome is shown in Table 2.
Embodiment 9:
The frequency sweep amplitude of ultrasonic treatment is ± 1.0kHz, remaining step is the same as embodiment 7；Tensile strength and elongation at break
Concrete outcome is shown in Table 2.
Embodiment 10:
The frequency sweep amplitude of ultrasonic treatment is ± 1.5kHz, remaining step is the same as embodiment 7；Tensile strength and elongation at break
Concrete outcome is shown in Table 2.
Embodiment 11:
The frequency sweep amplitude of ultrasonic treatment is ± 2.0kHz, remaining step is the same as embodiment 7；Tensile strength and elongation at break
Concrete outcome is shown in Table 2.
Influence of the different frequency sweep amplitudes of table 2 to composite membrane tensile strength and elongation at break
By composite membrane tensile strength and the elongation at break of comparative example 1 in table 2 and embodiment 7-11 it can be found that
(ultrasound is not added) compared with the control, the ultrasonic treatment of different frequency sweep amplitudes can make the tensile strength of composite membrane improve 9.2%-
23.7%, especially frequency sweep amplitude are that the ultrasonic treatment of ± 0.5kHz and ± 1.0kHz respectively improves the tensile strength of composite membrane
20.4% and 23.7%.Frequency sweep amplitude is being ultrasonically treated while also improving the disconnected of composite membrane for ± 0.5kHz and ± 1.0kHz
Elongation is split, 11.6% and 8.6% has been respectively increased.It is obtained by the above results, the tensile strength and fracture of comprehensive composite membrane
Elongation considers that frequency sweep amplitude is that the mechanical performance for the composite membrane that the ultrasonic treatment of ± 0.5kHz obtains is optimal.
Embodiment 12:
Tuna collagen-chitosan complex film preparation method of different pulse duty factor processing, according to following
Step carries out:
(1) collagen of certain mass is weighed in beaker, and the collagen for being configured to 2g/100mL with distilled water is molten
30min is dissolved in liquid, 50 DEG C of water-baths, and suction filtration obtains pure collagen solution.The chitosan of certain mass is weighed in beaker,
The glacial acetic acid that 2% (V/V) is added is made into the chitosan solution of 2g/100mL, and 50 DEG C of water-baths are dissolved 30min, stood overnight.By glue
Former albumen is mixed with chitosan solution according to mass ratio 1:4, and 25% (accounting for total soluble matters mass ratio) glycerol is added and makees plasticizer, and 20
10min is stirred under the conditions of DEG C is uniformly mixed so as to obtain mixed liquor.
(2) mixed liquor in step (1) is ultrasonically treated parameter are as follows: frequency in 55 DEG C of progress frequency sweep ultrasonic processing
28kHz；Power density 100W/L；Frequency sweep cycle 100ms；Frequency sweep amplitude ± 0.5kHz；Pulse duty factor 20%；Total time
10min.After ultrasonic treatment, mixed liquor is crosslinked 50min in 55 DEG C of water-bath.
(3) the ULTRASONIC COMPLEX film liquid that step (2) obtains is laid in clean polyethylene ware, is dried under the conditions of 40 DEG C
24h.It is taken out after drying, takes off film with blade after film is cooled to room temperature and obtain tuna collagen-chitosan complex film.
It saves it in (25 ± 0.5) DEG C, dry in the drier of relative humidity 58% or so equipped with being adjusted with saturation sodium bromide solution
2d measures the mechanical performance of composite membrane.
(4) Measuring Mechanical Properties of composite membrane:
The measurement of tensile strength (TS) and elongation at break (EAB): the smooth unabroken film of selection is simultaneously cut into 20mm
The strip of × 60mm measures its tensile strength and elongation at break with physical property instrument.Rate of extension is 60mm/min, and gauge length is
40mm。
Tensile strength calculation formula: TS=F/ (d × W)
In formula: TS-tensile strength (MPa)；The maximum tension (N) born when F-film fracture；D-film thickness (mm)；W—
Film width (mm).
Elongation at break calculation formula: EAB=(L-L0)×100/L0
In formula: EAB-elongation at break (%)；The distance between graticule (mm) when L-film fracture；L0The original graticule of-film
Distance (mm).
The concrete outcome of tensile strength and elongation at break is shown in Table 3.
Embodiment 13:
The pulse duty factor of ultrasonic treatment is 30%, remaining step is the same as embodiment 12；Tensile strength and elongation at break
Concrete outcome is shown in Table 3.
Embodiment 14:
The pulse duty factor of ultrasonic treatment is 50%, remaining step is the same as embodiment 12；Tensile strength and elongation at break
Concrete outcome is shown in Table 3.
Embodiment 15:
The pulse duty factor of ultrasonic treatment is 77%, remaining step is the same as embodiment 12；Tensile strength and elongation at break
Concrete outcome is shown in Table 3.
Embodiment 16:
The pulse duty factor of ultrasonic treatment is 90%, remaining step is the same as embodiment 12；Tensile strength and elongation at break
Concrete outcome is shown in Table 3.
The different pulse durations of table 3 compare the influence of composite membrane tensile strength and elongation at break
| Embodiment | Pulse duty factor % | Tensile strength MPa | Elongation at break % |
| Comparative example (i.e. embodiment 1) | Ultrasound is not added | 15.2 | 51.9 |
| Embodiment 12 | 20 | 15.8 | 53.9 |
| Embodiment 13 | 30 | 17.2 | 51.8 |
| Embodiment 14 | 50 | 16.6 | 52.4 |
| Embodiment 15 | 77 | 18.1 | 58.8 |
| Embodiment 16 | 90 | 17.6 | 56.2 |
It can be sent out by comparative example 1 in table 3 and the composite membrane tensile strength and elongation at break of embodiment 12-16
It is existing, (ultrasound is not added) compared with the control, the ultrasonic treatment of different pulse duty factors can be such that the tensile strength of composite membrane improves
The ultrasonic treatment that 3.9%-19.1%, especially ultrasound duty cycle are 77% and 90% respectively improves the tensile strength of composite membrane
19.1% and 15.8%.Same discovery, compared with the control, different ultrasound duty cycle processing also make the extension at break of composite membrane
Rate improves 0.9%-13.3%, and the ultrasonic treatment that wherein duty ratio is 77% improves the elongation at break of composite membrane most
It is more, reach 13.3%.It is obtained by the above results, the tensile strength and elongation at break of comprehensive composite membrane consider, pulse duration
The mechanical performance of the composite membrane obtained than the ultrasonic treatment for 77% is optimal.
It is obtained according to above-mentioned experimental result, it is (real that frequency sweep ultrasonic auxiliary prepares tuna collagen-chitosan complex film
Apply example 15) compared with the control (embodiment 1) that ultrasound is not added, tensile strength significantly improves 19.1%, and elongation at break is significant
Improve 13.3%, it follows that, the mechanical performance of composite membrane, which is significantly better than, after frequency sweep ultrasonic processing is not ultrasonically treated preparation
Composite membrane.
Claims (8)
1. tuna collagen-chitosan complex film frequency sweep ultrasonic preparation method, it is characterised in that as steps described below
It carries out:
(1) it prepares tuna collagen: the fish-skin after degreasing removing impurities albumen is soaked in solid-liquid ratio 1:70 (mg/mL)
In 0.5M acetic acid solution, the pepsin of 0.06% (W/V) 1800U/g pH=2, the homogeneous 5min in ice bath, 4 DEG C of enzymes are added
Solution extracts 48h, is centrifuged 45min in 4 DEG C of 10000r/min, supernatant is collagen crude extract；Collagen crude extract adds
NaCl to 0.9M saltouts overnight, and 6000r/min is centrifuged 20min, and gained precipitating is dissolved in 0.5M acetic acid, 10000r/min centrifugation
45min, gained supernatant add NaCl to 2.4M to saltout overnight, and 6000r/min is centrifuged 20min, and gained precipitating is dissolved in 0.5M second
In acid, dialyses three days, obtain collagen through vacuum freeze drying；
(2) tuna collagen-chitosan mixed liquor: the collagen that the step of weighing certain mass (1) obtains is prepared
In beaker, the collagen solution of 2g/100mL is configured to distilled water, 30min is dissolved in 50 DEG C of water-baths, and suction filtration obtains pure
Collagen solution；The chitosan of certain mass is weighed in beaker, the glacial acetic acid that 2% (V/V) is added is made into 2g/100mL
Chitosan solution, 50 DEG C of water-baths dissolve 30min, stand overnight；Collagen and chitosan solution are mixed according to mass ratio 1:4
It closes, and addition accounts for the glycerol that total soluble matters mass ratio is 25% and makees plasticizer, stirring 10min is uniformly mixed so as to obtain mixing under the conditions of 20 DEG C
Liquid；
(3) mixed liquor in step (2) is subjected to frequency sweep ultrasonic processing, obtains ULTRASONIC COMPLEX film liquid；It is ultrasonically treated parameter are as follows: frequency
Rate 28kHz；Power density 100W/L；20~500ms of frequency sweep cycle；Frequency sweep amplitude 0~± 2.0kHz；Pulse duty factor 20%~
90%；Total time 10min；After ultrasonic treatment, mixed liquor is crosslinked 50min in 55 DEG C of water-bath；
(4) composite membrane liquid that step (3) obtains is laid in clean polyethylene ware, is dried for 24 hours under the conditions of 40 DEG C；After drying
It takes out, takes off film with blade after film is cooled to room temperature and obtain tuna collagen-chitosan complex film.
2. the frequency sweep ultrasonic preparation method of tuna collagen-chitosan complex film according to claim 1, special
Sign is that wherein molecular weight of chitosan described in step (2) is 100,000 dalton.
3. the frequency sweep ultrasonic preparation method of tuna collagen-chitosan complex film according to claim 1, special
Sign is wherein frequency sweep ultrasonic frequency sweep cycle described in step (3) are as follows: 20,100,200,300,500ms.
4. the frequency sweep ultrasonic preparation method of tuna collagen-chitosan complex film according to claim 1, special
Sign is wherein frequency sweep ultrasonic frequency sweep amplitude described in step (3) are as follows: 0, ± 0.5, ± 1.0, ± 1.5, ± 2.0kHz.
5. the frequency sweep ultrasonic preparation method of tuna collagen-chitosan complex film according to claim 1, special
Sign be wherein frequency sweep ultrasonic pulse duty factor described in step (3) are as follows: 20% (10s/40s), 50% (10s/10s),
70% (10s/3s), 90% (24s/3s).
6. the frequency sweep ultrasonic preparation method of tuna collagen-chitosan complex film according to claim 3, special
Sign is that wherein frequency sweep ultrasonic frequency sweep cycle described in step (3) is 100ms.
7. the frequency sweep ultrasonic preparation method of tuna collagen-chitosan complex film according to claim 4, special
Sign is that wherein frequency sweep ultrasonic frequency sweep amplitude described in step (3) is ± 0.5kHz.
8. the frequency sweep ultrasonic preparation method of tuna collagen-chitosan complex film according to claim 5, special
Sign is wherein frequency sweep ultrasonic pulse duty factor described in step (3) are as follows: 70% (10s/3s).
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