CN111548441B - Ink melanin nanoparticle composite gel and preparation method thereof - Google Patents
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Abstract
The invention relates to an ink melanin nanoparticle composite gel and a preparation method thereof, wherein the method comprises the steps of freeze-drying and grinding ink into coarse ink powder; uniformly mixing the ink coarse powder with pure water, and homogenizing at 10000-20000 rpm for 5-15 min to obtain a black suspension; ultrasonically crushing black suspension liquid, centrifuging and freeze-drying to obtain ink fine powder; adding the ink fine powder, the high-molecular monomer and the clay into deionized water, and stirring for 10-20 min to obtain a treatment mixed solution; adding a catalyst and an initiator into the treated mixed solution, uniformly stirring, pouring into a template, and carrying out cross-linking polymerization for 0.5-2 h in an environment of 20-40 ℃ to obtain the ink melanin nanoparticle composite gel. According to the embodiment of the invention, the method can be used for preparing the uniform, stable, high-absorbance and high-strength ink natural melanin nanoparticle composite gel.
Description
Technical Field
The invention relates to the technical field of composite gels, in particular to an ink melanin nanoparticle composite gel and a preparation method thereof.
Background
The ink of cephalopodium organisms such as cuttlefish, squid and the like is black suspension sprayed when the cephalopodium organisms meet natural enemies, and the field of vision of the natural enemies can be disordered, so that people can escape. In the processing process, the ink belongs to leftovers and is usually discarded, so that great resource waste is caused. The ink mainly comprises natural melanin nano particles and a small amount of proteoglycan and the like, and the particles are in a relatively uniform spherical shape and have the diameter of about 100-200 nm. At present, scientists find that the cephalopodium biological ink not only has biological activities of antibiosis, anti-tumor, thermotherapy, hemostasis, antioxidation and the like, but also has great application potential in the field of functional materials such as photo-protection, heavy metal adsorption, energy storage, water treatment and the like as the ink nano particles serving as biodegradable natural melanin and is safer, nontoxic and pollution-free. However, the development of nano-particle functional materials of sepia is still in the spotlight, but the existing preparation method is single, and the stability and mechanical properties of the materials cannot meet the requirements of practical application, so that the design and development of novel and durable nano-particle functional materials of ink have urgent needs.
The hydrogel is used as a hydrophilic polymer carrier material with a three-dimensional network structure, has multiple responsiveness to the outside, and has wide application in the fields of biology, medicine, environment, energy and the like. By means of compounding, modifying, integrating and the like, multifunctional hydrogel composite materials are developed successively, such as sensors, artificial skin, seawater desalination, energy converters and the like, and become an important member of a new generation of intelligent materials. The novel hydrogel network compounded by the nanoparticles can play a synergistic function of the nanoparticles and the polymer network, and is one of important branches of functional hydrogel. At present, common nanoparticles comprise clay, silicon oxide, synthetic organic nanoparticles and the like, and a hydrogel network compounded by ink and natural melanin nanoparticles is not reported.
Disclosure of Invention
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art. Therefore, the invention aims to provide a preparation method of the ink melanin nanoparticle composite gel. According to the method, the ink nano particles, the inorganic nano particles and the polymer network are subjected to composite crosslinking through physical actions such as hydrogen bonds, static electricity and the like, so that the uniform, stable, high-absorbance and high-elasticity ink melanin nano particle composite gel is prepared, and the functions and the application fields of the ink natural melanin nano particle composite material are improved.
Therefore, in one aspect of the invention, the invention provides a preparation method of the ink melanin nanoparticle composite gel, which comprises the following steps:
(1) freeze-drying and grinding the ink into coarse ink powder without reflective particles;
(2) uniformly mixing the ink coarse powder and pure water according to the mass ratio of 1:20, and homogenizing at 10000-20000 rpm for 5-15 min to obtain a black suspension;
(3) carrying out ultrasonic cell crushing treatment on the black suspension, centrifuging and freeze-drying to obtain ink fine powder;
(4) adding the ink fine powder, the high-molecular monomer and the clay into deionized water, and stirring for 10-20 min to obtain a treatment mixed solution; wherein the mass ratio of the ink fine powder, the high molecular monomer, the clay and the deionized water is as follows: (0.001-0.02): 1, (0.5-2.0): 10;
(5) adding a catalyst and an initiator into the treated mixed solution, uniformly stirring, pouring into a template, and carrying out cross-linking polymerization for 0.5-2 h in an environment of 20-40 ℃ to obtain the ink melanin nanoparticle composite gel; wherein: the mass percentage of the catalyst in the mixed solution for treatment is 0.4-0.8%, and the mass percentage of the initiator in the mixed solution for treatment is 0.2-0.46%.
According to the preparation method of the ink melanin nanoparticle composite gel, the ink nanoparticles, the inorganic nanoparticles and the polymer network are subjected to composite crosslinking through physical actions such as hydrogen bonds, static electricity and the like, so that the uniform, stable, high-absorbance and high-elasticity ink natural melanin nanoparticle composite gel is prepared, and the functions and the application fields of the ink natural melanin nanoparticle composite material are improved; in addition, the preparation method is simple in preparation process, green and environment-friendly, and the swelling degree of the composite gel in water is 200-350%; the water-soluble polymer can exist stably in strong acid, and the swelling rate of the water-soluble polymer in hydrochloric acid with the pH value of 1 is 100-150%; the ultraviolet light transmittance is as low as 0-30%, and the infrared light transmittance is as low as 30-75%; the composite gel has excellent mechanical properties, the tensile strength of the composite gel can reach 180KPa, the elongation at break can reach more than 2000%, and the composite gel has great application potential in the fields of light protection, heavy metal adsorption, energy storage, water treatment and the like.
In addition, the preparation method of the ink melanin nanoparticle composite gel according to the embodiment of the present invention may further have the following additional technical features:
optionally, in step (3), the ultrasonic conditions are: the ultrasonic time is 10-20 min, the interval time of every ultrasonic time is 1-2s, and the power is 60-85%.
Optionally, in the step (4), the polymer monomer is one of acrylamide, isopropylacrylamide, N-dimethylacrylamide, acrylic acid, sodium acrylate, potassium acrylate, and 2-hydroxyethyl methacrylate.
Optionally, in step (4), the clay is a synthetic hectorite.
Alternatively, in step (5), the initiator is ammonium persulfate, potassium persulfate or sodium persulfate.
Optionally, in step (5), the catalyst is tetramethylethylenediamine.
In another aspect of the invention, the invention also provides an ink melanin nanoparticle composite gel, which is prepared by the preparation method.
According to the ink and melanin nanoparticle composite gel disclosed by the embodiment of the invention, the swelling degree in water can be 200-350% by adopting the method; the water-soluble polymer can exist stably in strong acid, and the swelling rate of the water-soluble polymer in hydrochloric acid with the pH value of 1 is 100-150%; the ultraviolet light transmittance is as low as 0-30%, and the infrared light transmittance is as low as 30-75%; the composite gel has excellent mechanical property, the tensile strength of the composite gel can reach 180KPa, and the elongation at break can reach more than 2000%.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
FIG. 1 is a scanning electron micrograph of the surface topography of fine particles of melanin nanoparticles of an ink prepared according to example 1 of the present invention;
FIG. 2 is a transmission electron micrograph of fine particles of melanin nanoparticles of an ink prepared according to example 1 of the present invention;
FIG. 3 is a representation of an ink melanin nanoparticle composite gel prepared in accordance with example 1 of the present invention;
FIG. 4 shows the swelling degree of the ink melanin nanoparticle composite gel prepared according to example 1 of the present invention in water;
FIG. 5 is a comparative illustration of soaking of the ink melanin nanoparticle composite gel prepared according to example 1 of the present invention in different solutions;
FIG. 6 is a full-band spectral absorption diagram of an ink melanin nanoparticle composite gel prepared according to example 1 of the present invention;
FIG. 7 is a schematic diagram of the mechanical properties of an ink melanin nanoparticle composite gel prepared according to example 1 of the present invention;
fig. 8 is a graph of the tensile strength of an ink melanin nanoparticle composite gel prepared according to example 1 of the present invention.
Detailed Description
The technical solution of the present invention is illustrated by specific examples below. It is to be understood that one or more method steps mentioned in the present invention do not exclude the presence of other method steps before or after the combination step or that other method steps may be inserted between the explicitly mentioned steps; it should also be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Moreover, unless otherwise indicated, the numbering of the various method steps is merely a convenient tool for identifying the various method steps, and is not intended to limit the order in which the method steps are arranged or the scope of the invention in which the invention may be practiced, and changes or modifications in the relative relationship may be made without substantially changing the technical content.
In order to better understand the above technical solutions, exemplary embodiments of the present invention are described in more detail below. While exemplary embodiments of the invention have been shown, it should be understood that the invention may be embodied in various forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
The test materials adopted by the invention are all common commercial products and can be purchased in the market.
The invention will now be described with reference to specific examples, which are intended to be illustrative only and not to be limiting in any way.
Example 1
In this example, the ink melanin nanoparticle composite gel was prepared by the following steps:
(1) manually stripping off the membrane of the cuttlefish ink sac, taking out the ink, freeze-drying by using a freeze dryer, grinding into coarse ink powder without reflective particles by using a mortar, and weighing 100g for later use;
(2) shaking and uniformly mixing the ink coarse powder and pure water according to the mass ratio of 1:20, and homogenizing for 15min at 20000rpm to obtain a uniform black suspension;
(3) after the black suspension is subjected to ultrasonic cell crushing treatment, centrifuging and freeze-drying at 8000rpm to obtain ink fine powder; in phase, the sonication conditions were: the ultrasonic time is 20min, the interval time is 2s every 2s of ultrasonic, and the power is 85 percent.
(4) Adding the ink fine powder, isopropyl acrylamide and synthetic hectorite laponite into deionized water, and stirring for 20min under a stirrer to obtain a treatment mixed solution; wherein the mass ratio of the ink fine powder, the acrylamide, the synthetic hectorite laponite and the deionized water is as follows: 0.02:1:2: 10;
(5) adding 0.8% of tetramethylethylenediamine and 0.4% of ammonium persulfate into the treated mixed solution, stirring uniformly, pouring into a template, carrying out cross-linking polymerization for 0.5h in the environment with the temperature of 40 ℃, and stripping the compound from the template to obtain the ink melanin nanoparticle composite gel.
Swelling the ink melanin nanoparticle composite gel in water, and measuring the swelling degree to be about 200%; stable in acid and the swelling rate was determined to be about 100% in hydrochloric acid at pH 1. The composite gel has high absorbance to full-wavelength light, the ultraviolet light transmittance is as low as 0 percent, and the infrared light transmittance is as low as 30 percent; the prepared composite gel is subjected to a tensile strength test, the tensile strength of the composite gel is 184KPa, and the elongation at break is about 2200%.
Example 2
In this example, the ink melanin nanoparticle composite gel was prepared by the following steps:
(1) manually stripping off the membrane of the cuttlefish ink sac, taking out the ink, freeze-drying by using a freeze dryer, grinding into coarse ink powder without reflective particles by using a mortar, and weighing 100g for later use;
(2) shaking and uniformly mixing the ink coarse powder and pure water according to the mass ratio of 1:20, and homogenizing for 5min under the condition of 10000rpm to obtain uniform black suspension;
(3) after the black suspension is subjected to ultrasonic cell crushing treatment, centrifuging and freeze-drying under the condition of 5000rpm to obtain ink fine powder; in phase, the sonication conditions were: the ultrasonic treatment time is 10min, the interval time is 1s every 1s of ultrasonic treatment, and the power is 60 percent.
(4) Adding the ink fine powder, acrylamide and synthetic hectorite laponite into deionized water, and stirring for 10min under a stirrer to obtain a treatment mixed solution; wherein the mass ratio of the ink fine powder, the acrylamide, the synthetic hectorite laponite and the deionized water is as follows: 0.001:1:0.5: 10;
(5) adding 0.4% of tetramethylethylenediamine and 0.2% of ammonium persulfate into the treated mixed solution, uniformly stirring, pouring into a template, carrying out cross-linking polymerization for 2 hours at the temperature of 20 ℃, and stripping the compound from the template to obtain the ink melanin nanoparticle composite gel.
Swelling the ink melanin nanoparticle composite gel in water, wherein the swelling degree is about 350%; stable in acid and the swelling rate was measured to be about 150% in hydrochloric acid at pH 1. The composite gel has high absorbance to full-wavelength light, the ultraviolet light transmittance is as low as 30%, and the infrared light transmittance is as low as 75%; the prepared composite gel is subjected to a tensile strength test, the tensile strength of the composite gel is 74KPa, and the elongation at break is about 2100%.
Example 3
In this example, the ink melanin nanoparticle composite gel was prepared by the following steps:
(1) manually stripping off a sac membrane of the squid ink sac, taking out ink, freeze-drying by using a freeze dryer, grinding into coarse ink powder without reflective particles by using a mortar, and weighing 50g for later use;
(2) shaking and uniformly mixing the ink coarse powder and pure water according to the mass ratio of 1:20, and homogenizing for 10min at 15000rpm to obtain a uniform black suspension;
(3) after the black suspension is subjected to ultrasonic cell crushing treatment, centrifuging and freeze-drying at 6000rpm to obtain ink fine powder; in phase, the sonication conditions were: the ultrasonic treatment time is 15min, the interval time is 2s every 2s of ultrasonic treatment, and the power is 70 percent.
(4) Adding the ink fine powder, isopropyl acrylamide and synthetic hectorite laponite into deionized water, and stirring for 15min under a stirrer to obtain a treatment mixed solution; wherein the mass ratio of the ink fine powder, the isopropyl acrylamide, the synthetic hectorite laponite and the deionized water is as follows: 0.01:1:1: 10;
(5) adding 0.6% of tetramethylethylenediamine and 0.3% of ammonium persulfate into the treated mixed solution, uniformly stirring, pouring into a template, carrying out cross-linking polymerization for 1h in the environment with the temperature of 30 ℃, and stripping the compound from the template to obtain the ink melanin nanoparticle composite gel.
Swelling the ink melanin nanoparticle composite gel in water, and measuring the swelling degree to be 300%; stable in acid and measured to have a swelling of about 120% in hydrochloric acid at pH 1. The composite gel has high absorbance to full-wavelength light, the ultraviolet light transmittance is as low as 10%, and the infrared light transmittance is as low as 50%; the prepared composite gel is subjected to a tensile strength test, the tensile strength of the composite gel is 150KPa, and the elongation at break is about 2100%.
Example 4
In this example, the ink melanin nanoparticle composite gel was prepared by the following steps:
(1) manually stripping off a sac membrane of the squid ink sac, taking out ink, freeze-drying by using a freeze dryer, grinding into coarse ink powder without reflective particles by using a mortar, and weighing 50g for later use;
(2) shaking and uniformly mixing the ink coarse powder and pure water according to the mass ratio of 1:20, and homogenizing for 15min at 20000rpm to obtain a uniform black suspension;
(3) after the black suspension is subjected to ultrasonic cell crushing treatment, centrifuging and freeze-drying at 8000rpm to obtain ink fine powder; in phase, the sonication conditions were: the ultrasonic time is 20min, the interval time is 2s every 2s of ultrasonic, and the power is 85 percent.
(4) Adding the ink fine powder, sodium acrylate and synthetic hectorite laponite into deionized water, and stirring for 20min under a stirrer to obtain a treatment mixed solution; wherein the mass ratio of the ink fine powder, the sodium acrylate, the synthetic hectorite laponite and the deionized water is as follows: 0.02:1:2: 10;
(5) adding 0.8% of tetramethylethylenediamine and 0.46% of ammonium persulfate into the treated mixed solution, stirring uniformly, pouring into a template, carrying out cross-linking polymerization for 2 hours at the temperature of 20 ℃, and stripping the compound from the template to obtain the ink melanin nanoparticle composite gel.
Swelling the ink melanin nanoparticle composite gel in water, and measuring the swelling degree to be 200%; stable in acid and the swelling rate was measured to be about 150% in hydrochloric acid at pH 1. The composite gel has high absorbance to full-wavelength light, the ultraviolet light transmittance is as low as 10%, and the infrared light transmittance is as low as 40%; the prepared composite gel is subjected to a tensile strength test, the tensile strength of the composite gel is 120KPa, and the elongation at break is about 2000%.
Example 5
In this example, the ink melanin nanoparticle composite gel was prepared by the following steps:
(1) manually stripping off the membrane of the cuttlefish ink sac, taking out the ink, freeze-drying by using a freeze dryer, grinding into coarse ink powder without reflective particles by using a mortar, and weighing 100g for later use;
(2) shaking and uniformly mixing the ink coarse powder and pure water according to the mass ratio of 1:20, and homogenizing for 15min under the condition of 10000rpm to obtain uniform black suspension;
(3) after the black suspension is subjected to ultrasonic cell crushing treatment, centrifuging and freeze-drying under the condition of 5000rpm to obtain ink fine powder; in phase, the sonication conditions were: the ultrasonic treatment time is 10min, the interval time is 1s every 1s of ultrasonic treatment, and the power is 85 percent.
(4) Adding the ink fine powder, 2-hydroxyethyl methacrylate and synthetic hectorite laponite into deionized water, and stirring for 20min under a stirrer to obtain a treatment mixed solution; wherein the mass ratio of the ink fine powder, the 2-hydroxyethyl methacrylate, the synthetic hectorite laponite and the deionized water is as follows: 0.01:1:1: 10;
(5) adding 0.46% of tetramethylethylenediamine and 0.6% of ammonium persulfate into the treated mixed solution, stirring uniformly, pouring into a template, carrying out cross-linking polymerization for 1h in the environment with the temperature of 40 ℃, and stripping the compound from the template to obtain the ink melanin nanoparticle composite gel.
Swelling the ink melanin nanoparticle composite gel in water, and measuring the swelling degree to be 200%; stable in acid and the swelling rate was determined to be about 100% in hydrochloric acid at pH 1. The composite gel has high absorbance to full-wavelength light, the ultraviolet light transmittance is as low as 20%, and the infrared light transmittance is as low as 65%; the prepared composite gel is subjected to a tensile strength test, the tensile strength of the composite gel is 80KPa, and the elongation at break is about 2000%.
In conclusion, the preparation process of the embodiment of the invention is simple, green and environment-friendly, and the swelling degree of the composite gel in water is 200-350%; stable in strong acid, swelling degree of 100-150% in hydrochloric acid with pH 1; the ultraviolet light transmittance is as low as 0-30%, and the infrared light transmittance is as low as 30-75%; the high-strength high-elongation polyethylene has excellent mechanical properties, the tensile strength can reach 180Kpa, the elongation at break can reach more than 2000%, and the high-strength high-elongation polyethylene has great application potential in the fields of light protection, heavy metal adsorption, energy storage, water treatment and the like.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above should not be understood to necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples described in this specification can be combined and combined by those skilled in the art.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (6)
1. A preparation method of the ink melanin nanoparticle composite gel is characterized by comprising the following steps:
(1) freeze-drying and grinding the ink into coarse ink powder without reflective particles;
(2) uniformly mixing the ink coarse powder and pure water according to the mass ratio of 1:20, and homogenizing at 10000-20000 rpm for 5-15 min to obtain a black suspension;
(3) carrying out ultrasonic cell crushing treatment on the black suspension, centrifuging and freeze-drying to obtain ink fine powder;
(4) adding the ink fine powder, the high-molecular monomer and the synthetic hectorite into deionized water, and stirring for 10-20 min to obtain a treatment mixed solution; wherein the mass ratio of the ink fine powder, the high molecular monomer, the clay and the deionized water is as follows: (0.001-0.02): 1, (0.5-2.0): 10;
(5) adding a catalyst and an initiator into the treated mixed solution, uniformly stirring, pouring into a template, and carrying out cross-linking polymerization for 0.5-2 h in an environment of 20-40 ℃ to obtain the ink melanin nanoparticle composite gel; wherein: the mass percentage of the catalyst in the mixed solution for treatment is 0.4-0.8%, and the mass percentage of the initiator in the mixed solution for treatment is 0.2-0.46%.
2. The method according to claim 1, wherein in the step (3), the ultrasonic conditions are: the ultrasonic treatment time is 10-20 min, the interval time of every ultrasonic treatment is 1-2s, and the power is 60-85%.
3. The method according to claim 1, wherein in the step (4), the polymer monomer is one of acrylamide, isopropylacrylamide, N-dimethylacrylamide, acrylic acid, sodium acrylate, potassium acrylate, and 2-hydroxyethyl methacrylate.
4. The production method according to claim 1, wherein in the step (5), the initiator is ammonium persulfate, potassium persulfate or sodium persulfate.
5. The method according to claim 1, wherein in the step (5), the catalyst is tetramethylethylenediamine.
6. An ink melanin nanoparticle composite gel prepared by the preparation method of any one of claims 1 to 5.
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| CN102167768A (en) * | 2010-12-22 | 2011-08-31 | 天津市志润德科技有限公司 | Super absorbent degradable colorful crystal soil containing nano-clay and preparation method thereof |
| WO2013180458A1 (en) * | 2012-05-29 | 2013-12-05 | 한국교통대학교 산학협력단 | Crosslinked hydrogel for drug delivery, and method for preparing the hydrogel |
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| CN102167768A (en) * | 2010-12-22 | 2011-08-31 | 天津市志润德科技有限公司 | Super absorbent degradable colorful crystal soil containing nano-clay and preparation method thereof |
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| CN104672407A (en) * | 2015-02-05 | 2015-06-03 | 西南林业大学 | Preparation method of natural melanin-acrylic acid composite superabsorbent resin |
| CN106009458A (en) * | 2016-06-20 | 2016-10-12 | 华南理工大学 | Novel pineapple peel residue cellulose-g-acrylic acid-kaolin-cuttlefish ink hydrogel and preparation method and application thereof |
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