CN105088538A - A preparation method of hydrophobic/super-hydrophobic protein coatings - Google Patents
A preparation method of hydrophobic/super-hydrophobic protein coatings Download PDFInfo
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Abstract
The invention relates to the technical field of amphoteric high molecular materials and provides a preparation method of hydrophobic/super-hydrophobic protein coatings. The method comprises the steps of weighing and taking zein and dissolving the zein in a alcohol-water solution and performing mixing treatment after a zein solution is formed, wherein the solubility of the zein solution is 50-400mg/ml; placing the zein solution in an injector of an electrostatic spinning apparatus for preparing hydrophobic/super-hydrophobic protein coatings. The method is simple in preparation process and low in preparation lost. The preparation speed is increased and the method is applicable to mass production.
Description
Technical field
The invention belongs to Amphiphatic high polymer field of material technology, particularly relate to a kind of preparation method of hydrophobic/super-hydrophobic protein coating.
Background technology
Hydrophobic material refers to the material that the water contact angle on surface is greater than 90 °, and super hydrophobic material refers to the material that the water contact angle on surface is greater than 150 °.Hydrophobic/superhydrophobic surfaces is generally obtained by two kinds of methods: improve surface roughness and reduce surface energy.Can be obtained by multiple method in the raising of nanometer and micro-meter scale lower surface roughness, such as photoetching technique, chemical etching, template, sol-gel synthesis, crystallization control, be separated, Electrospun, glycerol polymerization, layer-layer method, deposition and colloidal self-assembly etc.And the acquisition of low-surface-energy often needs surface chemistry coating to assist or surface molecular modification.Hydrophobic/super hydrophobic material uses fluorine-containing coat to reduce surface energy at present, and this material is expensive toxic effect not only, and biological concentration can cause environmental pollution in the environment.Molecular modification then relates to multi-step chemical reaction, takes time and effort, and does not meet the requirement of low energy consumption environmental protection.Super hydrophobic material synthesizes on various organic and inorganic material substrate, comprises macromolecular material, silicon wafer, sheet glass and sheet metal.But the substrate obtained is unsatisfactory, and their mechanical flexibility is very poor, and transparency and TENSILE STRENGTH are not high.
Electrostatic spinning a kind ofly utilizes polymer solution or melt to form injection stream under strong electric field thus carry out the technology of spinning process.In recent years, due to its superfine fibre process, Electrospun causes the concern of more and more people.The polymer that can carry out Electrospun processing at present in the world reaches 30 kinds, and comprising natural polymers such as DNA, collagen, silk-fibroins, and polyoxyethylene, polyacrylonitrile, nylon, polyvinyl alcohol, polyurethane, polycaprolactone etc. synthesize macromolecule.Compared with costliness, consuming time and be easy to produce the method polluted, this method can be reduced expenses and energy to a great extent.And at present owing to not having the guarantee of advanced electro-spinning equipment, the efficiency of electrostatic spinning suitability for industrialized production is extremely low, and want to utilize electrostatic spinning technique to reach high-speed production fiber coat, require extremely high to production equipment.
Summary of the invention
The object of the present invention is to provide a kind of environmental protection, cost low and the preparation method of hydrophobic/super-hydrophobic protein coating that production efficiency is high, being intended to solve prior art, to produce hydrophobic/super-hydrophobic protein coating high and production efficiency is low and the problem of hydrophobic/super-hydrophobic protein coating bad mechanical property that obtains to equipment requirement.
The present invention is achieved in that a kind of preparation method of hydrophobic/super-hydrophobic protein coating, comprises the following steps:
Taking zeins is dissolved in alcohol-water solution, and carry out mixing process after forming zein solution, the solubility of described zein solution is 50 ~ 400mg/ml;
The syringe described zein solution being placed in electrospinning device prepares hydrophobic/super-hydrophobic protein coating.
The preparation method of hydrophobic/super-hydrophobic protein coating provided by the invention, using Amphiphilic proteins zeins as raw material, electrostatic spinning technique is adopted to prepare hydrophobic/super-hydrophobic protein coating, first, the method does not need to carry out face coat and molecular modification, and therefore preparation process is simple, preparation cost is cheap; Secondly, the zeins of use is nontoxic, biodegradability and biocompatibility strong, there is the prospect of sustainable development, and hydrophobic/super-hydrophobic protein coating mechanical flexibility obtained is good; Again, use electrostatic spinning technique to prepare hydrophobic/super-hydrophobic protein coating, preparation speed is improved, thus makes to reduce the dependence of equipment, can be applicable to large-scale production.
Accompanying drawing explanation
Fig. 1 is spinning voltage that the embodiment of the present invention provides when being 18kV, and 50mg/ml zein solution prepares water contact angle and the SEM image of the hydrophobic coating of gained;
Fig. 2 is spinning voltage that the embodiment of the present invention provides when being 18kV, and 100mg/ml zein solution prepares water contact angle and the SEM image of the super-hydrophobic coat of gained;
Fig. 3 is spinning voltage that the embodiment of the present invention provides when being 18kV, and 150mg/ml zein solution prepares water contact angle and the SEM image of the super-hydrophobic coat of gained;
Fig. 4 is spinning voltage that the embodiment of the present invention provides when being 18kV, and 200mg/ml zein solution prepares water contact angle and the SEM image of the hydrophobic coating of gained;
Fig. 5 is spinning voltage that the embodiment of the present invention provides when being 18kV, and 250mg/ml zein solution prepares water contact angle and the SEM image of the hydrophobic coating of gained;
Fig. 6 is spinning voltage that the embodiment of the present invention provides when being 18kV is water contact angle and the SEM image that 300mg/ml zein solution prepares the hydrophobic coating of gained;
Fig. 7 is spinning voltage that the embodiment of the present invention provides when being 10kV is water contact angle and the SEM image that 100mg/ml zein solution prepares the hydrophobic coating of gained;
Fig. 8 is spinning voltage that the embodiment of the present invention provides when being 12kV is water contact angle and the SEM image that 100mg/ml zein solution prepares the hydrophobic coating of gained;
Fig. 9 is spinning voltage that the embodiment of the present invention provides when being 21kV is water contact angle and the SEM image that 100mg/ml zein solution prepares the hydrophobic coating of gained;
Figure 10 is spinning voltage that the embodiment of the present invention provides when being 18kV is the SEM image that 300mg/ml zein solution prepares the hydrophobic coating of gained;
Figure 11 is hydrophobic coating and the SEM image that zein solution that comparative example 1 provides prepares gained;
Figure 12 is hydrophobic coating and the SEM image that zein solution that comparative example 2 provides prepares gained.
Detailed description of the invention
In order to make the technical problem to be solved in the present invention, technical scheme and beneficial effect clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
No matter be in basic research or in the industry, super hydrophobic surface (SHS), because it is as the potential application of self-cleaning surface, as solar cell, windshield and stop-light, has caused increasing concern.SHS surface can also be antifouling, anti-biological pollution, antiseized and fire resistance characteristic.Although have numerous successful bionics fiber to realize super hydrophobic surface, the research of minority is only had to relate to the application of its potential biomaterial aspect.In view of this, embodiments provide a kind of preparation method of hydrophobic/super-hydrophobic protein coating, comprise the following steps:
S01. taking zeins is dissolved in alcohol-water solution, and carry out mixing process after forming zein solution, the solubility of described zein solution is 50 ~ 400mg/ml;
S02. the syringe described zein solution being placed in electrospinning device prepares hydrophobic/super-hydrophobic protein coating.
Particularly, in above-mentioned steps S01, described zeins is a kind of main protein in corn, is a kind of large biological molecule with good mechanical properties.Its rich content, cheapness, there is good biocompatibility, and be renewable resource.Meanwhile, described zeins is a kind of hydrophilic and natural amphoteric albumen that is hydrophobic grouping of simultaneously having.Study discovery through inventor, because zeins has special self-assembled structures characteristic, therefore, hydrophobic/super-hydrophobic protein coating adopting its preparation to be formed has good hydrophobic performance.The technology of hydrophobic or super-hydrophobic protein film is not also prepared at present with zeins.The embodiment of the present invention, by simple processing method, is that hydrophobic or super-hydrophobic protein film produced by material with zeins first, will be a method having very much the preparation of prospect alternative tradition super-hydrophobic.
In the embodiment of the present invention, described alcohol-water solution selects ethanol-water solution.Ethanol is the good innoxious solvent of volatility, is safe from harm to environment, adopts ethanol as lytic agent composition, be conducive in following electrostatic spinning technique, contribute to hydrophobic/super-hydrophobic albumen wire vent, therefore, require low to electrospinning device, thus form hydrophobic/super-hydrophobic albumen film uniformly.As preferred embodiment, described alcohol-water solution is the percent by volume of ethanol is the ethanol-water solution of 30 ~ 95%.As further preferred embodiment, described alcohol-water solution is the percent by volume of ethanol is the ethanol-water solution of 80 ~ 90%.Particularly when the percent by volume of ethanol in alcohol-water is 80% dissolving zeins, more contribute to wire vent.
Obtain zein solution after being dissolved by above-mentioned zeins, the concentration of described zein solution is 50 ~ 400mg/ml.This rational concentration range, effectively ensure that the hydrophobic property of hydrophobic/super-hydrophobic protein film and becomes fiber properties.As preferred embodiment, the concentration of described zein solution is 100 ~ 300mg/ml.
The above-mentioned zein solution configured fully is mixed process, until dissolution homogeneity is transparent.As preferred embodiment, the mixing processing method of described zein solution is for carry out ultrasonic process by zein solution, and ultrasonic time is 8 ~ 15min, and ultrasonic time is 10min more preferably.To of course it is to be understood that in this area that other modes that can reach fully mixing zein solution are also in the protection domain of the embodiment of the present invention.
In order to ensure zeins consistency, the process of above-mentioned steps S01 is preferably carried out at normal temperatures and pressures.
In above-mentioned steps S02, adopt electrostatic spinning to prepare hydrophobic/super-hydrophobic protein coating, want to reach suitability for industrialized production, ensure that final products become fiber properties simultaneously, high to the requirement of the unbridled machinery equipment of classics.Present inventor prepares the method for hydrophobic/super-hydrophobic protein coating through repeatedly studying and constantly bringing forth new ideas to electrostatic spinning, find: use zeins as raw material, as long as control the relevant parameter of electrospinning device well simultaneously, only need adopt general electrostatic spinning instrument equipment, just the object of hydrophobic/super-hydrophobic protein coating of high-speed production can be reached, speed can bring up to 20ml/h, and hydrophobic in preparation process/super-hydrophobic albumen wire vent is respond well, hydrophobic/super-hydrophobic protein coating obtained is uniformly fibrous under Electronic Speculum SEM, fibre diameter is at 0.7 ~ 1.2 micron.
In order to reach above-mentioned effect, as preferred embodiment.Prepare in the step of hydrophobic/super-hydrophobic protein coating at described electrostatic spinning, the voltage of described electrostatic spinning is 10 ~ 30kV, and electrostatic spinning speed is 0.5 ~ 20ml/h, and the spinning syringe needle of electrospinning device is 10 ~ 30cm to the distance of dash receiver.As further preferred embodiment, the voltage of described electrostatic spinning is 10 ~ 21kV, and the fltting speed of spinning solution is 0.5 ~ 10ml/h, and spinning syringe needle is 25cm to the distance of dash receiver.By arranging above-mentioned parameter, by zeins film-forming on reception electrostatic spinning apparatus.
Embodiment of the present invention application natural polymer replaces synthesizing compound, first, hydrophobic/super-hydrophobic coat is rapidly and efficiently prepared with the accessory substance zeins of corn wet processing, on the one hand, zeins cost is low, nontoxic, biodegradable, good biocompatibility, environmental protection, protects environment effectively, improves sustainable development; On the other hand, use amphiphilic zeins as raw material, avoid the step such as molecular modification and low surface energy coat, under the prerequisite of ensuring the quality of products, save production process, meanwhile, the amphiphatic molecule structure special due to zeins and self assembly characteristic, zeins fiber coat is prepared in rapid, high volume growth to use general electrospinning machine namely can accomplish, thus has greatly saved industrial production cost.Secondly, replace the existing method preparing super hydrophobic material with electrostatic spinning, make production method become easy steps from complexity simple, equipment requirement is low, and controllability is high, can be applicable to large-scale industrial production.And preparation speed can reach 20ml/h, effectively improves production efficiency.In addition, by embodiment of the present invention method prepare hydrophobic/super-hydrophobic coat hydrophobic performance is good, its water contact angle can reach 153 °, has self-cleaning function.
Be described below in conjunction with specific embodiment.
Embodiment 1
Under normal temperature and pressure (15 ~ 35 DEG C, 1 standard atmospheric pressure), take the zeins of 0.5g, be dissolved in the alcohol-water of 10ml80% (v/v), be configured to the solution of 50mg/ml, ultrasonic 10min, transparent to dissolution homogeneity.The solution configured is injected the syringe of electrospinning device, setting spinning voltage is 18kV, and the fltting speed of spinning solution is 0.2ml/h, and spinning syringe needle is 25cm to the distance of dash receiver.Film is prepared into by electrostatic spinning instrument.Preparing gained zeins hydrophobic coating to water contact angle is 138.2 °, and its water contact angle and SEM Electronic Speculum figure are as shown in Figure 1.
Embodiment 2
Under normal temperature and pressure (15 ~ 35 DEG C, 1 standard atmospheric pressure), take the zeins of 1.0g, be dissolved in the alcohol-water of 10ml80% (v/v), be configured to the solution of 100mg/ml, ultrasonic 10min, transparent to dissolution homogeneity.The solution configured is injected the syringe of electrospinning device, setting spinning voltage is 18kV, and the fltting speed of spinning solution is 0.2ml/h, and spinning syringe needle is 25cm to the distance of dash receiver.Film is prepared into by electrostatic spinning instrument.Preparing gained zeins super-hydrophobic coat to water contact angle is 153.6 °, and its water contact angle and SEM Electronic Speculum figure are as shown in Figure 2.
Embodiment 3
Under normal temperature and pressure (15 ~ 35 DEG C, 1 standard atmospheric pressure), take the zeins of 1.5g, be dissolved in the alcohol-water of 10ml80% (v/v), be configured to the solution of 150mg/ml, ultrasonic 10min, transparent to dissolution homogeneity.The solution configured is injected the syringe of electrospinning device, setting spinning voltage is 18kV, and the fltting speed of spinning solution is 0.2ml/h, and spinning syringe needle is 25cm to the distance of dash receiver.Film is prepared into by electrostatic spinning instrument.Preparing gained zeins super-hydrophobic coat to water contact angle is 150.4 °, and its water contact angle and SEM Electronic Speculum figure are as shown in Figure 3.
Embodiment 4
Under normal temperature and pressure (15 ~ 35 DEG C, 1 standard atmospheric pressure), take the zeins of 2.0g, be dissolved in the alcohol-water of 10ml80% (v/v), be configured to the solution of 200mg/ml, ultrasonic 10min, transparent to dissolution homogeneity.The solution configured is injected the syringe of electrospinning device, setting spinning voltage is 18kV, and the fltting speed of spinning solution is 0.2ml/h, and spinning syringe needle is 25cm to the distance of dash receiver.Film is prepared into by electrostatic spinning instrument.Preparing gained zeins hydrophobic coating to water contact angle is 143.8 °, and its water contact angle and SEM Electronic Speculum figure are as shown in Figure 4.
Embodiment 5
Under normal temperature and pressure (15 ~ 35 DEG C, 1 standard atmospheric pressure), take the zeins of 2.5g, be dissolved in the alcohol-water of 10ml80% (v/v), be configured to the solution of 250mg/ml, ultrasonic 10min, transparent to dissolution homogeneity.The solution configured is injected the syringe of electrospinning device, setting spinning voltage is 18kV, and the fltting speed of spinning solution is 0.2ml/h, and spinning syringe needle is 25cm to the distance of dash receiver.Film is prepared into by electrostatic spinning instrument.Preparing gained zeins hydrophobic coating to water contact angle is 141.0 °, and its water contact angle and SEM Electronic Speculum figure are as shown in Figure 5.
Embodiment 6
Under normal temperature and pressure (15 ~ 35 DEG C, 1 standard atmospheric pressure), take the zeins of 3.0g, be dissolved in the alcohol-water of 10ml80% (v/v), be configured to the solution of 300mg/ml, ultrasonic 10min, transparent to dissolution homogeneity.The solution configured is injected the syringe of electrospinning device, setting spinning voltage is 18kV, and the fltting speed of spinning solution is 0.2ml/h, and spinning syringe needle is 25cm to the distance of dash receiver.Film is prepared into by electrostatic spinning instrument.Preparing gained zeins hydrophobic coating to water contact angle is 136.4 °, and its water contact angle and SEM Electronic Speculum figure are as shown in Figure 6.
Embodiment 7
Under normal temperature and pressure (15 ~ 35 DEG C, 1 standard atmospheric pressure), take the zeins of 1.0g, be dissolved in the alcohol-water of 10ml80% (v/v), be configured to the solution of 100mg/ml, ultrasonic 10min, transparent to dissolution homogeneity.The solution configured is injected the syringe of electrospinning device, setting spinning voltage is 10kV, and the fltting speed of spinning solution is 0.2ml/h, and spinning syringe needle is 25cm to the distance of dash receiver.Film is prepared into by electrostatic spinning instrument.Preparing gained zeins hydrophobic coating to water contact angle is 130.5 °, and its water contact angle and SEM Electronic Speculum figure are as shown in Figure 7.
Embodiment 8
Under normal temperature and pressure (15 ~ 35 DEG C, 1 standard atmospheric pressure), take the zeins of 1.0g, be dissolved in the alcohol-water of 10ml80% (v/v), be configured to the solution of 100mg/ml, ultrasonic 10min, transparent to dissolution homogeneity.The solution configured is injected the syringe of electrospinning device, setting spinning voltage is 12kV, and the fltting speed of spinning solution is 0.2ml/h, and spinning syringe needle is 25cm to the distance of dash receiver.Film is prepared into by electrostatic spinning instrument.Preparing gained zeins hydrophobic coating to water contact angle is 131.2 °, and its water contact angle and SEM Electronic Speculum figure are as shown in Figure 8.
Embodiment 9
Under normal temperature and pressure (15 ~ 35 DEG C, 1 standard atmospheric pressure), take the zeins of 1.0g, be dissolved in the alcohol-water of 10ml80% (v/v), be configured to the solution of 100mg/ml, ultrasonic 10min, transparent to dissolution homogeneity.The solution configured is injected the syringe of electrospinning device, setting spinning voltage is 21kV, and the fltting speed of spinning solution is 0.2ml/h, and spinning syringe needle is 25cm to the distance of dash receiver.Film is prepared into by electrostatic spinning instrument.Preparing gained zeins hydrophobic coating to water contact angle is 139.4 °, and its water contact angle and SEM Electronic Speculum figure are as shown in Figure 9.
Embodiment 10
Under normal temperature and pressure (15 ~ 35 DEG C, 1 standard atmospheric pressure), take the zeins of 3.0g, be dissolved in the alcohol-water of 10ml80% (v/v), be configured to the solution of 300mg/ml, ultrasonic 10min, transparent to dissolution homogeneity.The solution configured is injected the syringe of electrospinning device, setting spinning voltage is 18kV, and the fltting speed of spinning solution is 10ml/h, and spinning syringe needle is 25cm to the distance of dash receiver.Film is prepared into by electrostatic spinning instrument.Prepare gained zeins hydrophobic coating fiberizing good, be 124.2 ° to water contact angle, its SEM Electronic Speculum figure as shown in Figure 10.
Comparative example 1
Zeins has film forming characteristics, and when zeins concentration is 300mg/ml, the water contact angle of the film obtained under air dry is 73 °, film smooth surface, and its SEM Electronic Speculum figure is as shown in Figure 11 as figure.
Comparative example 2
Under auto arrangement monolayer (SAM) helps, by evaporation-induced self-assembly (EISA) process, zeins can make hydrophobic membrane, and its water contact angle is 115 °, and its SEM Electronic Speculum figure is as shown in Figure 12 as figure.
By the comparison of water contact angle, known, electrostatic spinning technique substantially increases the hydrophobicity of maize alcohol-soluble protein film.Known by the scanning electron microscope image of different film, the fiber homogeneity that electrostatic spinning obtains is good, and aperture is little, and porosity is high.Adopt method described in comparative example 2 to prepare hydrophobic membrane, complex operation, and low concentration zein solution can only be used, film bad mechanical property.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (6)
1. a preparation method for hydrophobic/super-hydrophobic protein coating, is characterized in that, comprise the following steps:
Taking zeins is dissolved in alcohol-water solution, and carry out mixing process after forming zein solution, the solubility of described zein solution is 50 ~ 400mg/ml;
The syringe described zein solution being placed in electrospinning device prepares hydrophobic/super-hydrophobic protein coating.
2. the preparation method of hydrophobic/super-hydrophobic protein coating as claimed in claim 1, it is characterized in that, prepare in the step of hydrophobic/super-hydrophobic protein coating at described electrostatic spinning, the voltage of described electrostatic spinning is 10 ~ 30kV, electrostatic spinning speed is 0.5 ~ 20ml/h, and the spinning syringe needle of electrospinning device is 10 ~ 30cm to the distance of dash receiver.
3. the preparation method of hydrophobic/super-hydrophobic protein coating as claimed in claim 1, it is characterized in that, described alcohol-water solution is ethanol-water solution.
4. the preparation method of hydrophobic/super-hydrophobic protein coating as described in as arbitrary in claims 1 to 3, it is characterized in that, described alcohol-water solution is the percent by volume of ethanol is the ethanol-water solution of 30 ~ 95%.
5. the preparation method of hydrophobic/super-hydrophobic protein coating as described in as arbitrary in claims 1 to 3, it is characterized in that, described alcohol-water solution is the percent by volume of ethanol is the ethanol-water solution of 80 ~ 90%.
6. the preparation method of hydrophobic/super-hydrophobic protein coating as described in as arbitrary in claims 1 to 3, it is characterized in that, the mixing processing method of described zein solution is for carry out ultrasonic process by zein solution, and ultrasonic time is 8 ~ 15min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113969464A (en) * | 2021-11-15 | 2022-01-25 | 陕西科技大学 | Method for preparing novel zein nanofiber membrane by electrostatic spinning |
| CN115012227A (en) * | 2022-07-14 | 2022-09-06 | 江南大学 | Method for preparing hydrophobic textile by utilizing biomacromolecules |
| CN115233450A (en) * | 2022-08-04 | 2022-10-25 | 江南大学 | Method for preparing alcohol soluble protein hydrophobic finishing agent by biological method |
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| CN113969464A (en) * | 2021-11-15 | 2022-01-25 | 陕西科技大学 | Method for preparing novel zein nanofiber membrane by electrostatic spinning |
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