CN111229137A - Feather polypeptide modified polyacrylate fiber aerogel and preparation method and application thereof - Google Patents
Feather polypeptide modified polyacrylate fiber aerogel and preparation method and application thereof Download PDFInfo
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- CN111229137A CN111229137A CN202010036765.6A CN202010036765A CN111229137A CN 111229137 A CN111229137 A CN 111229137A CN 202010036765 A CN202010036765 A CN 202010036765A CN 111229137 A CN111229137 A CN 111229137A
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- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical group N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 20
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- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
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Images
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0202—Separation of non-miscible liquids by ab- or adsorption
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28047—Gels
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0092—Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
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- Environmental & Geological Engineering (AREA)
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Abstract
The invention discloses a feather polypeptide modified polyacrylate fiber aerogel and a preparation method and application thereof, which comprises the steps of firstly preparing a P (GMA-co-BA) polymer by adopting solution polymerization, simultaneously preparing feather polypeptide powder by carrying out absolute ethyl alcohol pretreatment, reduction treatment, alkaline hydrolysis and acid precipitation treatment on the feather, finally mixing the feather polypeptide powder and the feather polypeptide powder to prepare spinning solution, and preparing the feather polypeptide modified polyacrylate fiber aerogel with uniform diameter distribution and good appearance by electrostatic spinning; the prepared fiber aerogel has a micro-nano mesh structure, and a large number of active functional groups such as amino groups, epoxy groups, hydroxyl groups and the like are arranged on the surface of the fiber aerogel, so the fiber aerogel has wide application prospects in the fields of biological medicine, wastewater treatment, metal catalysts and the like.
Description
Technical Field
The invention relates to the technical field of polyacrylate aerogel preparation, in particular to a feather polypeptide modified polyacrylate fiber aerogel and a preparation method and application thereof.
Background
In recent years, marine oil spill accidents frequently occur, the pollution of water areas is becoming more serious, and particularly, the pollution of large and accumulated marine water areas caused by the discharge of industrial oil-containing waste water, oil ships and marine oil leakage not only causes serious threat to the living environment of marine organisms and human beings, but also causes the worry of people about the problem of cleaning the pollution. Therefore, the development of a novel oil absorption material with large adsorption capacity, high adsorption rate and good oil retention property is the main research direction for solving the problems at present.
The oil absorption material refers to a solid material which can collect oil from the water surface in an adhering and absorbing manner. The existing novel oil absorption material mainly comprises a natural oil absorption material, a super-hydrophobic oleophylic material, a carbon mesoporous material, porous aerogel, oil absorption foam, high-molecular oil absorption powder, hydrophobic oleophylic sponge and the like. These materials are generally divided into three major categories by source: natural organic oil absorption material, synthetic organic oil absorption material and inorganic oil absorption material.
In the process of research, the inventor of the application finds that the existing oil absorption material cannot achieve low price and high adsorbability at the same time.
Disclosure of Invention
In view of the above, the invention aims to provide a feather polypeptide modified polyacrylate fiber aerogel and a preparation method and application thereof, and is used for solving the problem that the existing oil absorption material cannot have low price and high absorption performance.
Based on the above purpose, the preparation method of the feather polypeptide modified polyacrylate fiber aerogel provided by the invention comprises the following steps:
synthesizing P (GMA-co-BA), dissolving butyl acrylate in N, N-dimethylformamide to obtain a butyl acrylate solution, adding glycidyl methacrylate and an initiator into the butyl acrylate solution in a crossed manner under the protection of nitrogen, and reacting for 7-15 h at 50-70 ℃ to obtain a P (GMA-co-BA) polymer;
preparing feather polypeptide, namely adding the feather into absolute ethyl alcohol for pretreatment, adding the pretreated feather into a reducing solution, reacting at the temperature of 60-100 ℃ for 0.5-5 h, filtering, washing, and freeze-drying; adding the feather polypeptide powder into alkali liquor, treating for 20-60 min at 80-130 ℃, filtering, carrying out acid precipitation on the filtrate until floccules are precipitated, and carrying out centrifugation, washing and vacuum drying to obtain feather polypeptide powder;
preparing modified polyacrylate fiber, blending feather polypeptide powder and P (GMA-co-BA) polymer to prepare a composite spinning solution, fully stirring the composite spinning solution for 18 to 30 hours by using a magnetic stirrer until the spinning solution is uniform and transparent, carrying out electrostatic spinning, and carrying out freeze drying to obtain the feather polypeptide modified polyacrylate fiber aerogel.
Optionally, the mass ratio of the butyl acrylate to the glycidyl methacrylate is 1: 2-10.
Optionally, the initiator is azobisisobutyronitrile, and the amount of the initiator is 0.1-0.8% of the total amount of the butyl acrylate and the glycidyl methacrylate.
Optionally, the concentration of the butyl acrylate solution is 20-80%.
Optionally, the reducing solution is a mixed solution of urea, sodium dodecyl benzene sulfonate and thioglycolic acid, and the concentration of the urea, the sodium dodecyl benzene sulfonate and the thioglycolic acid is 3-7: 1: 1.
Optionally, the alkali liquor is a sodium hydroxide solution with the concentration of 2-10 g/L.
Optionally, the acid solution of the acid precipitation is a hydrochloric acid solution with the pH value of 1-3.
Optionally, the feather polypeptide modified polyacrylate fiber aerogel comprises 5-13% of feather polypeptide powder by mass fraction.
Optionally, the voltage of the electrostatic spinning is 15-25 kV, the distance between the needle head and the receiving plate is 15-25 cm, the spinning speed is 0.1-0.5 mL/h, and the air humidity is 25-35%.
The feather polypeptide modified polyacrylate fiber aerogel is prepared by the preparation method; the feather polypeptide modified polyacrylate fiber aerogel is used in the fields of biological medicine, wastewater treatment and metal catalysts.
From the above, the preparation method of the feather polypeptide modified polyacrylate fiber aerogel provided by the invention adopts a solution polymerization method, uses Azobisisobutyronitrile (AIBN) as an initiator, uses Butyl Acrylate (BA) and Glycidyl Methacrylate (GMA) as monomers, and copolymerizes the monomers in N, N-Dimethylformamide (DMF) solvent to prepare copolymer P (GMA-co-BA); meanwhile, feather is subjected to absolute ethyl alcohol pretreatment, reduction treatment, alkaline hydrolysis and acid precipitation treatment in sequence to prepare feather polypeptide powder, and finally, composite nanofiber aerogel of feather polypeptide modified P (GMA-co-BA) polymer is prepared by electrostatic spinning, and the morphology and chemical composition of the composite nanofiber aerogel are represented by a scanning electron microscope and an infrared spectrum; the oil absorption performance of the composite nanofiber aerogel modified by the feather polypeptide is obviously improved, and the oil absorption multiplying power of the composite nanofiber aerogel is obviously increased along with the increase of the content of the feather polypeptide.
The feather polypeptide modified polyacrylate fiber aerogel prepared by the embodiment of the invention is in a micro-nano level, has a large specific surface area and is strong in adsorption capacity. The feather polypeptide powder modified polyacrylate nanofiber aerogel has a lower diameter and better biocompatibility, and the surface of the fiber aerogel has a large number of active functional groups such as amino groups, epoxy groups and hydroxyl groups, so that the feather polypeptide powder modified polyacrylate nanofiber aerogel has a very wide application prospect in the fields of biomedical treatment, wastewater treatment, metal catalysts and the like.
Drawings
FIG. 1 is a red light spectrum of a feather polypeptide modified polyacrylate fiber aerogel according to an embodiment of the present invention;
FIG. 2 is an SEM image of feather polypeptide modified polyacrylate fiber aerogel with different feather polypeptide contents according to the embodiment of the invention;
FIG. 3 is a thermogravimetric plot of P (GMA-co-BA) nanofiber aerogel and P (GMA-co-BA)/feather polypeptide composite nanofiber aerogel according to example of the present invention;
FIG. 4 is a graph of oil absorption rate of fiber aerogels with different feather polypeptide content according to the embodiment of the present invention;
FIG. 5 is a graph showing the relationship between the change of oil absorption rate of the fiber aerogel with different feather polypeptide content at different temperatures and time according to the embodiment of the invention.
Detailed Description
In the following description of the embodiments, the detailed description of the present invention, such as the manufacturing processes and the operation and use methods, will be further described in detail to help those skilled in the art to more fully, accurately and deeply understand the inventive concept and technical solutions of the present invention.
In order to solve the problem that the oil absorption material in the prior art cannot have low price and high adsorbability, the invention provides a preparation method of a feather polypeptide modified polyacrylate fiber aerogel, which comprises the following steps:
synthesizing P (GMA-co-BA), dissolving butyl acrylate in N, N-dimethylformamide to obtain a butyl acrylate solution, adding glycidyl methacrylate and an initiator into the butyl acrylate solution in a crossed manner under the protection of nitrogen, and reacting for 7-15 h at 50-70 ℃ to obtain a P (GMA-co-BA) polymer;
preparing feather polypeptide, namely adding the feather into absolute ethyl alcohol for pretreatment, adding the pretreated feather into a reducing solution, reacting at the temperature of 60-100 ℃ for 0.5-5 h, filtering, washing, and freeze-drying; adding the feather polypeptide powder into alkali liquor, treating for 20-60 min at 80-130 ℃, filtering, carrying out acid precipitation on the filtrate until floccules are precipitated, and carrying out centrifugation, washing and vacuum drying to obtain feather polypeptide powder;
preparing modified polyacrylate fiber, blending feather polypeptide powder and P (GMA-co-BA) polymer to prepare a composite spinning solution, fully stirring the composite spinning solution for 18 to 30 hours by using a magnetic stirrer until the spinning solution is uniform and transparent, carrying out electrostatic spinning, and carrying out freeze drying to obtain the feather polypeptide modified polyacrylate fiber aerogel.
Adopting a solution polymerization method, taking Azobisisobutyronitrile (AIBN) as an initiator, taking Butyl Acrylate (BA) and Glycidyl Methacrylate (GMA) as monomers, and copolymerizing in N, N-Dimethylformamide (DMF) solvent to prepare a copolymer P (GMA-co-BA); meanwhile, feather is sequentially subjected to absolute ethyl alcohol pretreatment, reduction treatment, alkaline hydrolysis and acid precipitation treatment to prepare feather polypeptide powder, and finally, composite nanofiber aerogel of feather polypeptide modified P (GMA-co-BA) polymer is prepared by electrostatic spinning, so that the composite nanofiber aerogel with low price and high adsorbability is prepared.
In some optional embodiments, in order to provide adsorbability to the composite nanofiber aerogel, the mass ratio of butyl acrylate to glycidyl methacrylate is 1: 2-10.
In some optional embodiments, in order to provide adsorbability to the composite nanofiber aerogel, the initiator is azobisisobutyronitrile, and the amount of the initiator is 0.1 to 0.8% of the total amount of the butyl acrylate and the glycidyl methacrylate.
In some optional embodiments, in order to provide adsorbability to the composite nanofiber aerogel, the concentration of the butyl acrylate solution is 20-80%.
In some optional embodiments, in order to provide adsorbability of the composite nanofiber aerogel, the reducing solution is a mixed solution of urea, sodium dodecyl benzene sulfonate and thioglycolic acid, and the concentration of the urea, the sodium dodecyl benzene sulfonate and the thioglycolic acid is 3-7: 1: 1.
In some optional embodiments, in order to provide the adsorbability of the composite nanofiber aerogel, the alkali solution is a sodium hydroxide solution with a concentration of 2-10 g/L.
In some optional embodiments, in order to provide adsorbability to the composite nanofiber aerogel, the acid solution for acid precipitation is a hydrochloric acid solution with a pH of 1-3.
In some optional embodiments, in order to provide adsorbability to the composite nanofiber aerogel, the feather polypeptide modified polyacrylate fiber aerogel comprises 5-13% of feather polypeptide powder by mass fraction.
In some optional embodiments, in order to provide adsorbability to the composite nanofiber aerogel, the voltage of electrostatic spinning is 15-25 kV, the distance between a needle and a receiving plate is 15-25 cm, the spinning speed is 0.1-0.5 mL/h, and the air humidity is 25-35%.
More specifically, in some alternative embodiments, the preparation method of the feather polypeptide modified polyacrylate fiber aerogel provided in embodiment 1 of the present invention includes the following steps:
synthesis of P (GMA-co-BA) binary copolymer, weighing 5.4g of BA in a flask, adding 48mL of DMF, fully dissolving, introducing nitrogen, adding 21.6g of GMA and 0.1575g of AIBN under the atmosphere of nitrogen, fully reacting in a water bath oscillator at 70 ℃, taking out after 10h, and placing in the shade.
More specific operation is as follows:
(1) weighing of solutions
The amount of AIBN used as an initiator is 0.5 percent (0.5 percent of the total mass of the monomers)
Mixing 28mL of DMF and 5.4g of BA, adding 10.8g of GMA after the BA is fully dissolved, and fully dissolving to obtain a solution a;
preparing an initiator solution from 12mL of DMF and 0.1575g of AIBN to obtain a solution b;
10mL of DMF and 0.8g of GMA were mixed and dissolved to obtain a solution c.
(2) Procedure for the preparation of the
Adding 4mL of the solution b into the solution a, filling nitrogen for 10-12 min, placing the solution in a constant-temperature water bath kettle at 70 ℃ for heating, and starting timing (starting synthesis);
after 1.5h, 5mL of solution c was added to solution a;
after 1.5h, 4mL of solution b was added to solution a;
after 1.5h, 5mL of solution c was added to solution a;
after 1.5h, add 4mL more solution b to solution a;
after 0.5h, the remaining solution b and solution c were all added to solution a and taken out after 10h of reaction (synthesis completed).
Preparing feather polypeptide, weighing 15g of feather, adding 500mL of absolute ethyl alcohol for pretreatment, washing the feather to be neutral by using distilled water, drying the feather, weighing 5g of the feather after pretreatment, shearing the feather into pieces, and adding the feather into a reduction treatment system consisting of 14g/L urea, 2g/L sodium dodecyl benzene sulfonate and 2g/L thioglycolic acid; stirring under the protection of nitrogen, reacting at 80 deg.C for 2 hr, filtering, washing, and freeze drying; adding into 6g/L sodium hydroxide solution at a bath ratio of 1:50, stirring and hydrolyzing at 100 deg.C for 40min, filtering the hydrolysate, acid-separating the filtrate with hydrochloric acid aqueous solution with pH of 2.0 until a large amount of floccule is separated out, centrifuging, washing, and vacuum drying to obtain feather polypeptide powder.
Preparing modified polyacrylate fiber, namely blending the feather polypeptide powder with a P (GMA-co-BA) binary copolymer according to the mass fractions of 5%, 7%, 10% and 13% (the mass fraction of the copolymer is occupied by the feather polypeptide powder) to prepare a composite spinning solution, and fully stirring the composite spinning solution for 24 hours by using a magnetic stirrer until the spinning solution is uniform and transparent; transferring 4mL of the prepared spinning solution into an injector with the capacity of 5mL, horizontally placing the injector on a propeller, adjusting the spinning voltage to be 18kV, adjusting the spinning speed to be 0.3mL/h, and carrying out electrostatic spinning at the ambient temperature of 26 ℃ and the air humidity of 30% in the spinning process. And (5) freezing and drying to obtain the feather polypeptide modified polyacrylate fiber aerogel.
First, performance test
1. Preparing P (GMA-co-BA) nano-fiber aerogel by electrostatic spinning, taking DMF as a solvent, weighing 10g P (GMA-co-BA) copolymer, dissolving in a proper amount of DMF solvent, preparing a spinning solution, and fully stirring for 24 hours by using a magnetic stirrer until the spinning solution is uniform and transparent. 4mL of the prepared spinning solution was taken into a syringe having a capacity of 5mL, and the syringe was horizontally placed on a propeller. The spinning voltage is adjusted to be 18kV, and the spinning speed is 0.3 mL/h. The electrostatic spinning is carried out at the ambient temperature of 26 ℃ and the air humidity of 30 percent in the spinning process. And (5) after freeze drying, obtaining the P (GMA-co-BA) nanofiber aerogel.
2. Performance test of P (GMA-co-BA)/feather polypeptide composite nanofiber aerogel
(1) Infrared spectroscopy
And respectively carrying out infrared spectroscopy on the P (GMA-co-BA) nanofiber aerogel and the feather polypeptide modified P (GMA-co-BA) composite nanofiber aerogel through a Fourier transform infrared spectrometer.
Fourier infrared spectroscopy (FT-IR): the method is characterized in that the sample of the fiber aerogel is measured by a potassium bromide tabletting method, and the scanning range is 4000-400 cm-1。
As shown in figure 1, the FT-IR spectrum of the P (GMA-co-BA)/feather polypeptide composite nanofiber aerogel is shown. As can be seen in the infrared spectrogram of feather polypeptide (FIG. 1a), 3309cm-1The absorption peak of (1) is O-H stretching vibration, 1658cm-1、1533cm-1、1234cm-1The absorption peaks of the stretching vibration of (a) are classified into an amide i band (C ═ O bond stretching vibration), an amide ii band (N-H bond stretching vibration), and an amide iii band (C-N bond stretching vibration). As can be seen in the infrared spectrum of the P (GMA-co-BA) fiber aerogel (FIG. 1b), 915cm-1、851cm-1Is a stretching vibration absorption peak of an epoxy group; 1744cm-1、1165cm-1Characteristic absorption peaks of ester carbonyl and ether bond respectively; 2924cm-1、2866cm-1Are respectively-CH2、—CH3The characteristic absorption peak of (A) was measured, and a P (GMA-co-BA) copolymer was obtained by solution polymerization. As can be seen from the infrared spectrogram (figure 1c) of the P (GMA-co-BA)/feather polypeptide composite nanofiber aerogel, after the P (GMA-co-BA) and the feather polypeptide are blended, the comparison curve b is 3550-3365 cm-1A wider and stronger-OH characteristic absorption peak appears, 1693-1635 cm-1The peak is the stretching vibration peak of ester carbonyl in P (GMA-co-BA) and carbonyl in the amide I band in the feather, and in addition, the characteristic absorption peak of epoxy group is weakened, which shows that the epoxy group in the composite nanofiber aerogel reacts with the primary amine group on the polypeptide of the feather. Infrared analysis shows that P (GMA-co-BA)/feather polypeptide composite nanofiber aerogel is successfully prepared in the embodiment of the invention.
(2) SEM characterization
Respectively characterizing the P (GMA-co-BA) nanofiber aerogel and the feather polypeptide modified P (GMA-co-BA) composite nanofiber aerogel.
Scanning Electron Microscope (SEM): according to the testing requirements of a scanning electron microscope, 5 samples are respectively prepared from P (GMA-co-BA) nanofiber aerogel and feather polypeptide modified P (GMA-co-BA) composite nanofiber aerogel, 20-second gold spraying treatment is respectively carried out on the surfaces of the samples to be tested, and the surface morphology of the samples is observed by adopting the scanning electron microscope. Selecting 50 fibers with clear outlines, and observing the changes of the shapes and diameters of the fibers before and after modification.
As shown in fig. 2, (a), (b), (c) and (d) in fig. 2 are SEM images of the composite nanofiber aerogel containing feather polypeptide powder in the amounts of 0%, 5%, 7% and 10%, respectively. With the increase of the content of the feather polypeptide, the viscosity of the spinning solution is gradually increased, because the feather polypeptide contains a large amount of hydroxyl and amino, more hydrogen bonds can be formed among the molecules of the spinning solution, the entanglement among molecular chains is promoted, and the viscosity of the spinning solution is increased. The higher the viscosity and the higher the surface tension, the lower the spinning droplet splitting capacity and therefore the polymer solution concentration and the fiber diameter increase.
As can be seen from the figure, as the polypeptide content of the feather increases, the fiber diameter decreases first and then increases. When the content of feather polypeptide is 5% (as shown in FIG. 2b), fiber is entangled, the fiber diameter is reduced but the thickness is uneven, and spindle-shaped 'beads' exist; when the content of feather polypeptide is 7% (as shown in fig. 2c), the viscosity of the spinning solution becomes a dominant factor influencing the polymer morphology, the fiber diameter is increased, and the thickness is not uniform; when the content of feather polypeptide is increased to 10% (as shown in fig. 2d), the viscosity of the spinning solution is high, the fibers are crosslinked and intertwined to form fiber knots, and the diameter of the fibers is obviously increased. In addition, when the content of the feather polypeptide is 13%, the viscosity of the spinning solution is too high, so that the solution is condensed at a spinneret orifice due to less solvent and easy volatilization, and the needle head is easy to block.
(3) Thermogravimetric analysis (TGA)
Measuring the relation between the mass and the temperature of the sample at a programmed temperature by using a microcomputer differential thermal balance to research the thermal stability of the sampleQualitative, temperature rise rate 10 deg.C/min, N2And (4) measuring in an atmosphere.
FIG. 3 is a thermogravimetric analysis diagram of P (GMA-co-BA) nanofiber aerogel and P (GMA-co-BA)/feather polypeptide composite nanofiber aerogel. From fig. 3a, it can be seen that the initial decomposition temperature (temperature corresponding to 10% weight loss) of the P (GMA-co-BA) nanofiber aerogel is 307 ℃, which may be caused by evaporation of water molecules in the fiber aerogel. When the temperature is higher than 307 ℃, the P (GMA-co-BA) nanofiber aerogel starts to be decomposed continuously, the decomposition rate is accelerated continuously along with the increase of the temperature, the decomposition rate does not start to have a descending trend until 420 ℃, and the P (GMA-co-BA) nanofiber aerogel is decomposed basically and completely when the temperature reaches 470 ℃. From fig. 3b, it can be seen that the initial decomposition temperature of the P (GMA-co-BA)/feather polypeptide composite nanofiber aerogel is 316 ℃, the decomposition rate continuously increases with the increase of the temperature, and the composite nanofiber aerogel is not substantially completely decomposed until 570 ℃. The comparison of the two results shows that: the thermal stability of the P (GMA-co-BA)/feather polypeptide composite nanofiber aerogel is higher than that of the P (GMA-co-BA) nanofiber aerogel, which is probably because after the feather polypeptide is added, the epoxy groups in the fiber and the primary amine groups in the feather polypeptide are crosslinked, so that the thermal stability of the composite nanofiber is improved.
(4) Oil absorption test
Two samples of about 0.01g are cut and weighed as W1Then using tweezers to hold the sample and quickly immerging the sample into normal temperature oil, taking out the sample by a glass rod at certain time intervals, weighing W after the surface oil is drained2And the oil absorption multiplying power is recorded as Q, the oil absorption multiplying power is shown as the formula (1):
oil absorption tests are respectively carried out on the P (GMA-co-BA) nanofiber aerogel and the P (GMA-co-BA)/feather polypeptide composite nanofiber aerogel, and the influence of temperature on the P (GMA-co-BA) nanofiber aerogel and the P (GMA-co-BA)/feather polypeptide composite nanofiber aerogel is researched. Standing at room temperature, 40 deg.C, 60 deg.C and 80 deg.C for 1 hr, measuring oil absorption at 1min, 5min, 10min, 30min, 1 hr, 3 hr, 12 hr and 24 hr, and drawing oil absorption curve.
According to the embodiment of the invention, the oil absorption performance of the sample is researched mainly according to two influence factors of temperature and the content of feather polypeptide.
(1) Effect of feather polypeptide content on oil absorption of samples
FIG. 4 is a graph showing the relationship between the oil absorption multiplying power of the composite nanofiber aerogel with different feather polypeptide contents at room temperature (28 ℃) and the time, wherein graphs a-d are oil absorption curves of the composite nanofiber aerogel with the feather polypeptide contents of 0%, 5%, 7% and 10%, respectively. It can be seen from the figure that the oil absorption rate is very fast in the early stage of adsorption and slowly decreases in the later stage until the absorption is balanced. And with the increase of the content of the feather polypeptide, the oil absorption multiplying power of the composite nanofiber aerogel is obviously higher than that of the pure nanofiber aerogel, when the content of the feather polypeptide is 7%, the oil absorption multiplying power of the composite nanofiber aerogel reaches 6130%, and the oil absorption multiplying power of the pure nanofiber aerogel is only about 1800%. The particle size of the emulsified oil is in the range of 0.1-10 mu m, the emulsified oil belongs to an oil-in-water type, and the P (GMA-co-MA)/feather polypeptide composite nanofiber is hydrophobic fiber except for the advantages of large specific surface area, high porosity and the like of the composite nanofiber aerogel. For oil-absorbing materials, the hydrophobicity and lipophilicity of the material are key factors influencing the oil-absorbing performance of the material. With the addition of feather polypeptide, the crosslinking degree of the composite nanofiber aerogel is increased, and the filling power is improved, so that the adsorption performance of the composite nanofiber aerogel is improved. It can also be seen from the figure that the pure fiber aerogel when the content of feather polypeptide is 0% reaches the adsorption balance in about 1h, and the composite nanofiber aerogel with the feather polypeptide accounting for 7% reaches the adsorption balance after 7h, which is mainly because the former can only adsorb on the surface of the fiber aerogel, the time required by the adsorption balance is short, and the latter requires a long time for the adsorption balance due to the crosslinking of the fiber aerogel.
(2) Effect of temperature on oil absorption of samples
Fig. 5 is a graph of the oil absorption rate of the fiber aerogel with different feather polypeptide contents at different temperatures as a function of time, wherein graphs (a) - (d) are oil absorption curves of the fiber aerogel with the feather polypeptide contents of 0%, 5%, 10% and 7% at different temperatures respectively. As can be seen from the figure, when the content of the feather polypeptide is the same, the oil absorption multiplying power of the fiber aerogel is gradually reduced along with the increase of the temperature; when the temperature is the same, the oil absorption multiplying power of the fiber aerogel is increased and then reduced along with the increase of the polypeptide content of the feather; when the temperature rises, the thermal motion of molecules is intensified, the intermolecular force is weakened, the combination of hydrogen bonds, Van der Waals force and other chemical bonds is reduced, the hydrophobicity of the fiber aerogel is reduced, and meanwhile, the internal structure of feather polypeptide is damaged due to the rise of the temperature, so that the oil absorption multiplying power is reduced; and when the temperature is the same, the content of the feather polypeptide is increased, so that the bulkiness of the fiber aerogel is improved, and the adsorption capacity of the fiber aerogel is improved. It can be seen from the figure that the oil absorption rates of different fiber aerogels are very fast in the initial stage of adsorption, and all the fiber aerogels reach saturated adsorption after 7 h. The oil absorption of the composite nanofiber aerogel with the feather polypeptide content of 10% is obviously higher than that of the pure nanofiber aerogel, the oil absorption rate of the pure fiber aerogel is only 1508% at 40 ℃, and the oil absorption rate of the composite nanofiber aerogel (with the feather polypeptide content of 7%) reaches 4762%.
Comparing fig. 4, it can be concluded that: the oil absorption performance of the composite nanofiber aerogel is obviously superior to that of the pure nanofiber aerogel. When the content of the feather polypeptide is the same, the oil absorption multiplying power of the fiber aerogel is gradually reduced along with the rise of the temperature; when the temperature is the same, the oil absorption multiplying power of the fiber aerogel is increased and then reduced along with the increase of the polypeptide content of the feathers. At room temperature (28 ℃), when the content of feather polypeptide is 7%, the oil absorption multiplying power of the composite nanofiber aerogel is the maximum, and reaches 6130%.
(5) Mechanical Property test
The thickness and the width of the sample are measured and recorded, then the sample is cut into the size of 1cm multiplied by 3cm, the sample is processed for 1h at 40 ℃, 60 ℃ and 80 ℃ respectively and then is tested on a single fiber strength tester with the measuring range of 500cN, three groups of samples are measured, the average value is taken, and the breaking strength is shown as the formula (2).
The mechanical property of the sample is researched mainly according to two influence factors of temperature and the content of feather polypeptide.
(1) Influence of feather polypeptide content on mechanical properties of sample
Table 1 shows the mechanical properties of the fiber aerogel with different feather polypeptide contents at room temperature (28 ℃), and it can be seen from the table that the breaking strength of the P (GMA-co-BA) nanofiber aerogel is 13.17MPa, the breaking elongation is 167.4%, when 5% of feather polypeptide is added, the breaking strength of the fiber aerogel is increased to 13.45MPa, the breaking elongation is reduced to 146.8%, and along with the increase of the feather polypeptide content, the breaking strength of the fiber aerogel is increased firstly and then reduced, and the breaking elongation is reduced gradually.
TABLE 1 mechanical properties of fibrous aerogels with different feather polypeptide contents
According to structural analysis, with the increase of the polypeptide content of the feather, the diameters of the prepared composite nano fibers are reduced, the contact area between the fibers is increased, the structure of the composite nano fiber aerogel is made to be more compact, the friction force between the fibers is increased, and the relative slippage between the fibers is reduced, so that the breaking strength of the composite nano fiber aerogel is increased, and the breaking elongation is reduced; on the molecular level, the breaking of the polymer mainly breaks 3 forms of intramolecular chemical bonds, intermolecular hydrogen bonds and van der waals force, and intermolecular slippage. With the addition of the feather polypeptide, the epoxy group on P (GMA-co-BA) and the primary amine group on the feather polypeptide are crosslinked to form a stronger covalent bond, and the breaking strength of the fiber aerogel is continuously increased; when the content of the feather polypeptide reaches a certain value, plasticization is generated, so that the binding force between covalent bonds is weakened, and the breaking strength is reduced when the content of the feather polypeptide reaches 10%. Meanwhile, as part of feather polypeptide molecules are embedded between the P (GMA-co-BA) macromolecular chain segments, the P (GMA-co-BA) macromolecular chain segments cannot be well stretched in the stretching process, so that the breaking elongation of the composite nanofiber aerogel is reduced.
(2) Influence of temperature on mechanical Properties of samples
The mechanical properties of the fiber aerogel at different temperatures are shown in tables 2-5, and the data in the comparative analysis table can be known as follows: when the content of the feather polypeptide is the same, the breaking strength of the fiber aerogel is reduced and the breaking elongation is increased along with the increase of the temperature; when the temperature is the same, the breaking strength of the fiber aerogel is increased and then reduced along with the increase of the polypeptide content of the feather, and the breaking elongation is reduced. This is mainly because, at an elevated temperature, the thermal movement of the molecules is increased and the intermolecular forces are weakened, so that the breaking strength is reduced and the elongation at break is increased. When the content of the feather polypeptide is increased, the epoxy group on P (GMA-co-BA) and the primary amine group on the feather polypeptide are crosslinked to form a stronger covalent bond, so that the relative slippage between fibers is reduced, the breaking strength of the composite nanofiber aerogel is increased, and the breaking elongation is reduced; when the content of the feather polypeptide is 10%, the breaking strength of the fiber aerogel is reduced because the diameter of the fiber is increased, and macromolecular chains playing a main role in the fiber aerogel are relatively reduced, so that the breaking strength of the fiber aerogel is reduced.
TABLE 2 mechanical Properties of pure nanofiber aerogels at different temperatures
TABLE 3 mechanical properties of composite nanofiber aerogel at different temperatures when the feather polypeptide content is 5%
TABLE 4 mechanical properties of composite nanofiber aerogel at different temperatures when the feather polypeptide content is 7%
TABLE 5 mechanical properties of composite nanofiber aerogel at different temperatures with feather polypeptide content of 10%
Comparing table 1, it can be seen that: the mechanical property of the composite nanofiber aerogel is superior to that of the pure nanofiber aerogel. When the content of the feather polypeptide is the same, the breaking strength of the fiber aerogel is reduced and the breaking elongation is increased along with the increase of the temperature; when the temperature is the same, the breaking strength of the fiber aerogel is increased and then reduced along with the increase of the polypeptide content of the feather, and the breaking elongation is reduced. When the temperature is 40 ℃ and the content of feather polypeptide is 7%, the breaking strength of the nanofiber aerogel is the maximum and reaches 39.90MPa, and the breaking elongation of the fiber aerogel is 151.4%.
Those of ordinary skill in the art will understand that: the discussion of any embodiment above is meant to be exemplary only, and is not intended to intimate that the scope of the disclosure, including the claims, is limited to these examples; within the idea of the invention, also features in the above embodiments or in different embodiments may be combined, steps may be implemented in any order, and there are many other variations of the different aspects of the invention as described above, which are not provided in detail for the sake of brevity.
The embodiments of the invention are intended to embrace all such alternatives, modifications and variances that fall within the broad scope of the appended claims. Therefore, any omissions, modifications, substitutions, improvements and the like that may be made without departing from the spirit and principles of the invention are intended to be included within the scope of the invention.
Claims (10)
1. The preparation method of the feather polypeptide modified polyacrylate fiber aerogel is characterized by comprising the following steps:
synthesizing P (GMA-co-BA), dissolving butyl acrylate in N, N-dimethylformamide to obtain a butyl acrylate solution, adding glycidyl methacrylate and an initiator into the butyl acrylate solution in a crossed manner under the protection of nitrogen, and reacting for 7-15 h at 50-70 ℃ to obtain a P (GMA-co-BA) polymer;
preparing feather polypeptide, namely adding the feather into absolute ethyl alcohol for pretreatment, adding the pretreated feather into a reducing solution, reacting at the temperature of 60-100 ℃ for 0.5-5 h, filtering, washing, and freeze-drying; adding the feather polypeptide powder into alkali liquor, treating for 20-60 min at 80-130 ℃, filtering, carrying out acid precipitation on the filtrate until floccules are precipitated, and carrying out centrifugation, washing and vacuum drying to obtain feather polypeptide powder;
preparing the feather polypeptide modified polyacrylate fiber aerogel, blending feather polypeptide powder and a P (GMA-co-BA) polymer to prepare a composite spinning solution, fully stirring the composite spinning solution for 18 to 30 hours by using a magnetic stirrer until the spinning solution is uniform and transparent, carrying out electrostatic spinning, and carrying out freeze drying to obtain the feather polypeptide modified polyacrylate fiber aerogel.
2. The preparation method of the feather polypeptide modified polyacrylate fiber aerogel of claim 1, wherein the mass ratio of the butyl acrylate to the glycidyl methacrylate is 1: 2-10.
3. The preparation method of the feather polypeptide modified polyacrylate fiber aerogel of claim 1, wherein the initiator is azobisisobutyronitrile, and the amount of the initiator is 0.1-0.8% of the total amount of the butyl acrylate and the glycidyl methacrylate.
4. The preparation method of the feather polypeptide modified polyacrylate fiber aerogel of claim 1, wherein the concentration of the butyl acrylate solution is 20-80%.
5. The preparation method of the feather polypeptide modified polyacrylate fiber aerogel according to claim 1, wherein the reducing solution is a mixed solution of urea, sodium dodecyl benzene sulfonate and thioglycolic acid, and the concentration of the urea, the sodium dodecyl benzene sulfonate and the thioglycolic acid is 3-7: 1: 1.
6. The preparation method of the feather polypeptide modified polyacrylate fiber aerogel according to claim 1, wherein the alkali solution is a sodium hydroxide solution with a concentration of 2-10 g/L.
7. The preparation method of the feather polypeptide modified polyacrylate fiber aerogel according to claim 1, wherein the acid solution for acid precipitation is a hydrochloric acid solution with a pH value of 1-3.
8. The preparation method of the feather polypeptide modified polyacrylate fiber aerogel of claim 1, wherein the feather polypeptide modified polyacrylate fiber aerogel comprises 5-13% of feather polypeptide powder by mass.
9. The preparation method of the feather polypeptide modified polyacrylate fiber aerogel according to claim 1, wherein the electrostatic spinning voltage is 15-25 kV, the distance between a needle head and a receiving plate is 15-25 cm, the spinning speed is 0.1-0.5 mL/h, and the air humidity is 25-35%.
10. A feather polypeptide modified polyacrylate fiber aerogel is characterized by being prepared by the preparation method of any one of claims 1-9; the feather polypeptide modified polyacrylate fiber aerogel is used in the fields of biological medicine, wastewater treatment and metal catalysts.
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| CN108579699A (en) * | 2018-04-17 | 2018-09-28 | 北京科技大学 | Adsorb the three-dimensional manometer fiber sponge sorbing material and preparation method of bacterial endotoxin |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117344404A (en) * | 2023-10-27 | 2024-01-05 | 安徽工程大学 | Polypeptide ion conductive fiber based on polymerizable deep eutectic solvent, preparation and application |
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