CN107459662A - A kind of preparation method of Nanometer composite hydrogel - Google Patents
A kind of preparation method of Nanometer composite hydrogel Download PDFInfo
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- CN107459662A CN107459662A CN201710796464.1A CN201710796464A CN107459662A CN 107459662 A CN107459662 A CN 107459662A CN 201710796464 A CN201710796464 A CN 201710796464A CN 107459662 A CN107459662 A CN 107459662A
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- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
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Abstract
The present invention relates to a kind of preparation method of Nanometer composite hydrogel, belong to hydrogel preparing technical field.The preparation method of Nanometer composite hydrogel provided by the invention, comprises the following steps：1) chitin that degree of acetylation is 0.94 is subjected to acidolysis, obtains chitin nano whisker enhancing agent dispersing liquid；2) chitin nano whisker enhancing agent dispersing liquid is mixed with gelatin solution, cooling obtains Nanometer composite hydrogel.The Nanometer composite hydrogel good mechanical property that preparation method of the present invention obtains, gelling temperature is high, has fabulous stability in the environment of highly acid and high salt ionic concentration, can be widely used in edible cosmetic product and field of medicaments.
Description
Technical field
The present invention relates to hydrogel preparing technical field, and in particular to a kind of preparation method of Nanometer composite hydrogel.
Background technology
Hydrogel is three-dimensional polymerization networking, can absorb the substantial amounts of moisture of maintenance, is widely used in food, cosmetics,
Biomedicine field, and bone tissue and medicine load.Hydrogel needs high intensity and flexibility in application, and reversible
Deformation behavior.However, the polyalcohol hydrogel of general chemistry crosslinking is frangible under a certain pressure, it is easily broken.Cross-linked hydrogel, it is double
Network aqueous gel and Nanometer composite hydrogel are common hydrogel.Mechanical performance of the prior art to the above-mentioned hydrogel of enhancing
Studied.Wherein, research has shown that double-network hydrogel can strengthen the mechanical performance of gel, but these most of polymer
Hydrogel needs to add the reinforcing agent of high concentration, is unsuitable for food industry.At present, a variety of crosslinking agents (glutaraldehyde, turn
Glutaminase, and Geniposide etc.) gelatin hydrogel is applied to by the method for crosslinking, in order to strengthen gelatin hydrogel
Mechanical performance, but there is the problem of potential toxicity and high consumption in these crosslinking agents.
The content of the invention
It is an object of the invention to provide a kind of preparation method of Nanometer composite hydrogel.What preparation method of the present invention obtained
Nanometer composite hydrogel good mechanical property, gelling temperature is high, has in the environment of highly acid and high salt ionic concentration fabulous
Stability, edible cosmetic product and field of medicaments can be widely used in.
The invention provides a kind of preparation method of Nanometer composite hydrogel, comprise the following steps：
1) chitin that degree of acetylation is 0.94 is subjected to acidolysis, obtains chitin nano whisker enhancing agent dispersing liquid；
2) chitin nano whisker enhancing agent dispersing liquid is mixed with gelatin solution, cooling obtains Nanometer composite hydrogel.
Preferably, the step 1) acidolysis uses hydrochloric acid solution or sulfuric acid solution
Preferably, the temperature of the step 1) acidolysis is 80~120 DEG C.
Preferably, the time of the step 1) acidolysis is 2~16h.
Preferably, the mass concentration of gelatin is 10~14% in the step 2) gelatin solution.
Preferably, addition of step 2) the chitin nano whisker reinforcing agent in gelatin solution be 0.25~
1%w/v.
Preferably, the temperature of the step 2) mixing is 40~60 DEG C.
Preferably, the temperature of the step 2) cooling is 4~14 DEG C.
Preferably, the time of the step 2) cooling is 12~24h.
Preferably, the source of chitin includes shrimp shell, crab shell and insect shell.
The invention provides a kind of preparation method of Nanometer composite hydrogel.The present invention is by preparing nano-chitosan whisker
And then Nanometer composite hydrogel is prepared, nano-chitosan crystal whisker preparation method is simple, and raw material sources enrich, cheap, has
Preferable biocompatibility；Less nano-chitosan whisker can be prepared, these nano-chitosan whiskers can fill
Into gelatin substrate, interacted with gelatin, prepare Nanometer composite hydrogel；Obtained hydrogel has higher mechanicalness
Energy and gelling temperature, and the acid and alkali-resistance and salt tolerance having had.In food, medicine and cosmetic field have good answer
With.
Brief description of the drawings
The nano-chitosan that Fig. 1 provides for the embodiment of the present invention 4, gelatin hydrogel, the projection electricity of Nanometer composite hydrogel
Mirror figure；Wherein：A, b is nano-chitosan；C is gelatin hydrogel；D is Nanometer composite hydrogel；
Fig. 2 is the zeta potential diagrams of the gelatin solution that inventive embodiments 4 provide and chitin suspension；Wherein：A is gelatin
Solution；B is nano-chitosan；
The nano-chitosan that Fig. 3 provides for inventive embodiments 4, gelatin, Nanometer composite hydrogel infrared spectrogram；
Fig. 4 is the scanning electron microscope (SEM) photograph of the Nanometer composite hydrogel for the various concentrations nano-chitosan that inventive embodiments 4 provide；
Fig. 5 is the temperature scanning figure of the Nanometer composite hydrogel for the various concentrations nano-chitosan that inventive embodiments 4 provide
And gelling temperature curve map；
Fig. 6 is the frequency scanning figure of the Nanometer composite hydrogel for the various concentrations nano-chitosan that inventive embodiments 4 provide；
Fig. 7 is that the compression stress of the Nanometer composite hydrogel for the various concentrations nano-chitosan that inventive embodiments 4 provide should
Varied curve figure；
Fig. 8 is that the compression stress of the Nanometer composite hydrogel for the various concentrations nano-chitosan that inventive embodiments 4 provide should
Varied curve figure difference maximum compression ratio；
Fig. 9 is the Nanometer composite hydrogel swelling curve figure for the various concentrations nano-chitosan that inventive embodiments 4 provide；
Figure 10 is the frequency scanning of the Nanometer composite hydrogel of the nano-chitosan for the different pH that inventive embodiments 4 provide
Figure；
Figure 11 is the frequency of the Nanometer composite hydrogel of the nano-chitosan for the different salt ionic concentrations that inventive embodiments 4 provide
Rate scanning figure.
Embodiment
The invention provides a kind of preparation method of Nanometer composite hydrogel, comprise the following steps：
1) chitin that degree of acetylation is 0.94 is subjected to acidolysis, obtains chitin nano whisker enhancing agent dispersing liquid；
2) chitin nano whisker enhancing agent dispersing liquid is mixed with gelatin solution, cooling obtains Nanometer composite hydrogel.
The chitin that degree of acetylation is 0.94 is carried out acidolysis by the present invention, obtains chitin nano whisker reinforcing agent.At this
In invention, the step 1) acidolysis uses hydrochloric acid solution or sulfuric acid solution.When choosing hydrochloric acid solution progress acidolysis, the crust
The quality of element and the volume ratio of hydrochloric acid solution are 1g：30mL, the molar concentration of the hydrochloric acid solution is preferably 3mol/L；Work as use
When sulfuric acid solution carries out acidolysis, the quality of chitin and the volume ratio of sulfuric acid solution are 1g：30mL, mole of the sulfuric acid solution
Concentration is preferably 3mol/L.In the present invention, the temperature of the acidolysis is 80~120 DEG C, more preferably 95 DEG C.In the present invention
In, the time of the acidolysis is 2~16h, more preferably 8~12h, most preferably 10h.In the present invention, the acid hemolysis process
Preferably include to dialyse afterwards, centrifuge washing and the step dried.The present invention does not have special limitation to the condition of the dialysis, uses
Dialysis process well known to those skilled in the art, centrifugation washing, dialysis of the present invention are preferably carried out after present invention dialysis
The pH of dispersion liquid that act as, by the acid removal in dispersion liquid, making with centrifugation washing is neutrality.The present invention washes to the centrifugation
Method there is no special restriction, using it is well known to those skilled in the art centrifugation wash operating condition.It is of the present invention
It is preferably freeze drying process to dry, and the present invention does not have special restriction to the lyophilized condition, ripe using those skilled in the art
The lyophilisation condition known.
After obtaining chitin nano whisker reinforcing agent, chitin nano whisker is strengthened the present invention into agent dispersing liquid and gelatin is molten
Liquid mixes, and cooling obtains Nanometer composite hydrogel.In the present invention, in institute's gelatine solution the mass concentration of gelatin for 10~
14%, more preferably 12%.In the present invention, addition of the chitin nano whisker reinforcing agent in gelatin solution is
0.25~1%w/v, more preferably 0.5~0.7%w/v.In the present invention, the temperature of the mixing is 40~60 DEG C, more preferably
For 55 DEG C.In the present invention, the temperature of the cooling is 4~14 DEG C, more preferably 10~12 DEG C.In the present invention, it is described cold
But time is 12~24h, more preferably 15~20h, the effect of heretofore described cooling be in order that gelatin forms gel,
In cooling procedure, interaction of hydrogen bond occurs with nano-chitosan for gelatin and electrostatic interaction forms gel.
The present invention does not have special restriction to the source of the chitin, and in the present invention, the source of chitin is preferably wrapped
Include shrimp shell, crab shell and insect shell.
A kind of preparation method of Nanometer composite hydrogel of the present invention is done further with reference to specific embodiment
Detailed introduction, technical scheme include but is not limited to following examples.
Embodiment 1
1st, chitin nano whisker enhancing agent dispersing liquid：Chitin and hydrochloric acid that degree of acetylation is 0.94 are pressed into 1g：30mL
Mixing, acidolysis temperature are 95 DEG C, time 10h, and acidolysis obtains chitin nano whisker enhancing agent dispersing liquid.Acid hemolysis process is laggard
Row dialysis, centrifugation are washed and dried.
2nd, Nanometer composite hydrogel：Chitin nano whisker enhancing agent dispersing liquid is prepared into various concentrations, is added to 14%
Gelatin solution (45 DEG C) in, both are well mixed, and final nano-chitosan accounts for the 0.25% of whole solution, 0.5% He
1.0%, then mixed liquor is placed under conditions of 4 DEG C and cools down 12h, obtain Nanometer composite hydrogel.In addition to research acid-base value
With influence of the ion concentration to composite aquogel, it is used to adjust pH value to 3.0,4.0,5.0,7.0,8.0 with 1MNaOH or HCl
Or 9.0, with NaCl adjustment ion concentration be 10,30,50,70,90mM.
Embodiment 2
Gelling temperature and viscoelastic measure：The dynamic rheological property measurement of Nanometer composite hydrogel is controllable using straining
Rheometer measurement, arrange parameter：Temperature is 25 DEG C, and root diameter is 50mm and 1mm respectively with parallel sheet separation, frequency scans and is
Angular frequency range 0.1-100rad/s, constant strain are 1% (in Linear Viscoelastic Region), record storage modulus (G ') and loss
Modulus (G ").In order to observe the maturing of gel sample, time sweep is measured, and 2.5h is scanned under the conditions of 10 DEG C.Temperature scanning
When from 40 DEG C drop to 10 DEG C, then increasing to 40 DEG C with 1 DEG C per minute of speed.
Embodiment 3
1st, the measure of mechanical performance：Pour Nanometer composite hydrogel into a diameter of 20mm, in height 10mm mould, place
12h under the conditions of 4 DEG C.TPA tests, recording parameters hardness (g), elasticity, cohesion, stickiness (g), chewing are carried out with food texture measurement
(g) it is and restorative.
Measurement is compressed to hydrogel using food texture measurement.One water-setting blob (length:20mm, width:10mm,
Highly:20mm) it is placed on relatively low plate, the whole surface of gel sample is covered with P36R probes, with 1mm/s judgement of speed change
Rate is compressed.Stress and stress data are have recorded in experiment.Cyclic test is also carried out passing through repeated compression.
2nd, the measure of swelling character：The swelling character of Nanometer composite hydrogel is studied and calculated, and according to
Lower formula calculates:
Swellbility=(W-Wd)/Wd × 100 (1)
These samples soak 24h in phosphate buffer solution, and measure weight in wet base (W).Then, with measurement after freeze-drying
Dry weight (Wd).
Embodiment 4
1st, the microstructure and infrared spectrum analysis of nano-chitosan and composite aquogel
Fig. 1 is nano-chitosan, gelatin hydrogel and the projection electron microscope of Nanometer composite hydrogel in the present invention.Note：Figure
A, scheme b：Nano-chitosan；Scheme c：Gelatin hydrogel；Scheme d:Nanometer composite hydrogel
Fig. 2 is the zeta potential diagrams of gelatin solution and chitin suspension.Note：a：Gelatin solution；b：Nano-chitosan.
Fig. 3 is nano-chitosan, gelatin, Nanometer composite hydrogel infrared spectrogram of the present invention.
Fig. 4 is the scanning electron microscope (SEM) photograph of the Nanometer composite hydrogel of various concentrations nano-chitosan in invention.
The explanation of Fig. 1~3, acid-hydrolyzed nano-chitosan average length are 300nm, a diameter of 20nm, in the aqueous solution and bright
The dispersiveness having had in sol solution, does not assemble.Infrared spectrum shows nano-chitosan with gelatin in composite aquogel
Interaction of hydrogen bond in matrix be present.Fig. 4 illustrates that scanning electron microscope (SEM) photograph shows with the increase of addition nano-chitosan concentration, gel
Aperture is gradually reduced, and the quantity in hole gradually increases, and forms close network structure.By infrared spectrum it is demonstrated experimentally that proving
Interaction of hydrogen bond be present with nano-chitosan in gelatin.
2nd, influence of the various concentrations nano-chitosan to gelatin gel temperature and viscoelasticity
Fig. 5 is the temperature scanning figure and gelling temperature of the Nanometer composite hydrogel of various concentrations nano-chitosan in invention
Curve map.
Fig. 6 is the frequency scanning figure of the Nanometer composite hydrogel of various concentrations nano-chitosan in invention.
Fig. 5~6 illustrate, with the gradual increase of nano-chitosan concentration, gelling temperature increase, when addition is
When 0.5%, gelling temperature and melting temperature are maximum, and viscoplasticity also gradually increases.Frequency scanning result shows, when addition nanometer
When the concentration of chitin is 0.5%, the modulus of elasticity of composite aquogel adds 42.4%.It is solidifying to show that nano-chitosan adds
The viscoplasticity of glue.
3rd, influence of the various concentrations nano-chitosan to gelatin mechanical performance and swelling character
Fig. 7 is the compression stress strain curve figure of the Nanometer composite hydrogel of various concentrations nano-chitosan in invention.
Fig. 8 be invention in various concentrations nano-chitosan Nanometer composite hydrogel compression stress strain curve figure not
Same maximum compression ratio.
Fig. 9 is the Nanometer composite hydrogel swelling curve figure of various concentrations nano-chitosan in invention.
Table 1 is influence of the various concentrations nano-chitosan to the texture characteristic of Nanometer composite hydrogel, with reference to Fig. 7~9 and
Table 1 illustrates that addition nano-chitosan increases gel strength, analyzes, can draw by TPA, with nano-chitosan concentration
Increase, the hardness of composite aquogel, chewiness and viscosity gradually increase, and when addition is 1.0%, hardness is pure gelatin hardness
1.5%.Compression experiment shows after adding nano-chitosan that the stress required for destroying gelatin increases, and when addition is
When 0.5%, required power is maximum.Shown by swellability experiment, the addition of nano-chitosan, the swelling for reducing gelatin is special
Property, indicate the high-mechanical property of Nanometer composite hydrogel and low swelling character.
Influence of the various concentrations nano-chitosan of table 1 to the texture characteristic of Nanometer composite hydrogel
4th, influence of the sensitive environment (salt ion, pH etc.) to composite aquogel
Figure 10 is the frequency scanning figure of the Nanometer composite hydrogel of different pH nano-chitosan in invention.
Figure 11 is the frequency scanning figure of the Nanometer composite hydrogel of the nano-chitosan of different salt ionic concentrations in invention
Figure 10~11 illustrate that Nanometer composite hydrogel shows high energy storage mould under different PH and salt ionic concentration
Amount, and gelatin of the composite aquogel prepared under strong acid, highly basic and high salt ionic concentration than being prepared under the same terms
Modulus of elasticity it is big, show that composite aquogel has preferable salt tolerant, strong alkali-acid resistance.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of Nanometer composite hydrogel, comprises the following steps：
1) chitin that degree of acetylation is 0.94 is subjected to acidolysis, obtains chitin nano whisker enhancing agent dispersing liquid；
2) chitin nano whisker enhancing agent dispersing liquid is mixed with gelatin solution, cooling obtains Nanometer composite hydrogel.
2. preparation method according to claim 1, it is characterised in that the step 1) acidolysis uses hydrochloric acid solution or sulfuric acid
Solution.
3. preparation method according to claim 1, it is characterised in that the temperature of the step 1) acidolysis is 80~120 DEG C.
4. preparation method according to claim 1, it is characterised in that the time of the step 1) acidolysis is 2~16h.
5. preparation method according to claim 1, it is characterised in that the quality of gelatin is dense in the step 2) gelatin solution
Spend for 10~14%.
6. preparation method according to claim 1 or 5, it is characterised in that step 2) the chitin nano whisker enhancing
Addition of the agent in gelatin solution is 0.25~1%w/v.
7. preparation method according to claim 1, it is characterised in that the temperature of step 2) mixing is 40~60 DEG C.
8. the preparation method according to claim 1 or 7, it is characterised in that the temperature of the step 2) cooling is 4~14
℃。
9. the preparation method according to claim 1 or 8, it is characterised in that the time of the step 2) cooling for 12~
24h。
10. according to the preparation method described in Claims 1 to 4 any one, it is characterised in that the source of chitin includes shrimp
Shell, crab shell and insect shell.
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| CN114672173A (en) * | 2022-04-24 | 2022-06-28 | 罗赛洛(温州)明胶有限公司 | Water-absorbing gelatin sponge and preparation method thereof |
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| CN109897194B (en) * | 2019-01-29 | 2021-09-21 | 南京林业大学 | Preparation method of high-strength hydrogel imitating insect epidermis structure |
| CN114672173A (en) * | 2022-04-24 | 2022-06-28 | 罗赛洛(温州)明胶有限公司 | Water-absorbing gelatin sponge and preparation method thereof |
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