CN110923838B - High-light-guiding and high-moisture-retention nano composite hydrogel optical fiber and preparation method thereof - Google Patents
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Abstract
The invention relates to a high-light-guiding and high-moisture-preserving nano composite hydrogel optical fiber and a preparation method thereof, wherein the preparation method comprises the following steps: the raw material component system is obtained by in-situ polymerization and synchronous stretching. The obtained material has good light guide performance, flexibility and various environment adaptability. The invention not only obviously improves the multiple performances of the hydrogel optical fiber, but also has the advantages of easily obtained raw materials required by preparation, simple process, great industrial production potential and hopeful application to biosensing devices in various environments.
Description
Technical Field
The invention belongs to the field of preparation of functional composite hydrogel optical fibers, and particularly relates to a high-light-guiding and high-moisture-retention nano composite hydrogel optical fiber and a preparation method thereof.
Background
The optical fiber sensor has the advantages of good inherent safety, small electromagnetic interference and high insulation strength, and can effectively avoid the influence of external electromagnetic signal interference. However, the conventional optical fiber materials are limited to hard glass or plastic, and although the optical fiber materials have good light transmission capability, the optical fiber materials cannot be suitable for flexible and complex human body deformation, so that the application of the optical fiber materials in the field of novel wearable equipment is limited.
The hydrogel is a colloidal material formed by crosslinking hydrophilic macromolecules in water, is soft and tough, and has better deformability. The optical fiber material can bear large elongation, bending and pressure deformation after being processed into the optical fiber material. The sodium alginate/PEGDA gel optical fiber prepared by foreign researchers through a template method not only is long in preparation time, but also is extremely easy to dehydrate and difficult to use for a long time. Other existing methods are also based on a template method to prepare the gel optical fiber, but are limited by complex processing modes and factors which are easily influenced by the environment, and the currently reported hydrogel optical fiber cannot meet the requirements of actual production and application.
CN103408683A discloses a physical/chemical crosslinked photothermal response hydrogel, which is difficult to be processed into hydrogel fibers after molding due to its internal highly crosslinked three-dimensional network structure.
CN105592865A discloses a method for preparing hydrogel optical fiber by ultraviolet radiation, which can have high uniformity and transparency. However, the prepared hydrogel fiber is easily affected by the environment, and the hydrogel fiber absorbs water or loses water, so that the hydrogel fiber deforms. In order to overcome the problems that the hydrogel optical fiber is difficult to process due to a cross-linked network and the prepared hydrogel optical fiber is easily influenced by the environment, the invention can prepare the high-light-guiding and high-moisture-retention nano composite hydrogel optical fiber.
Disclosure of Invention
The invention aims to solve the technical problem of providing a high-light-guiding and high-moisture-preserving nano composite hydrogel optical fiber and a preparation method thereof, which overcome the problems of complex processing means, weak mechanical strength, easy dehydration and the like of the hydrogel optical fiber in the prior art, and the invention adopts a polymerization-stretching synchronous preparation method.
The invention relates to a nano-composite hydrogel optical fiber which is obtained by in-situ polymerization and synchronous stretching of a system containing the following components; wherein the reaction system comprises the following components: solvent, inorganic cross-linking agent, high light transmittance monomer and initiator, and reacting and copolymerizing at normal temperature; wherein the solvent is a mixture of water and glycerol.
And (2) pre-polymerizing a pre-polymerization solution consisting of a solvent, inorganic nano particles and a gel monomer in a tube, reacting for a certain time to form a primary hydrogel which has certain continuity but is not completely reacted, and stretching, orienting and shaping the primary hydrogel in the in-situ polymerization process until the cross-linked structure becomes compact and the appearance becomes uniform, thus obtaining the hydrogel.
The inorganic cross-linking agent is lithium bentonite Laponite and/or silicon dioxide; the high light-transmitting monomer is acrylamide AAm and oligoethylene glycol methyl ether methacrylate OEGMA; the initiator is one or more of potassium persulfate, ammonium persulfate and sodium persulfate; the system also comprises an accelerator; wherein the accelerator is one of N, N, N ', N' -tetramethyl ethylenediamine and N, N-dimethylaniline.
The invention relates to a preparation method of a nano composite hydrogel optical fiber, which comprises the following steps:
(1) uniformly mixing an inorganic cross-linking agent, a solvent, a high-light-transmittance monomer and an initiator to obtain a gel pre-polymerization solution;
(2) and adding an accelerator into the gel prepolymerization solution, transferring the gel prepolymerization solution into a reaction tube for prepolymerization reaction, extruding primary hydrogel which does not form a complete network in the reaction tube after the reaction is carried out for 3-20min, synchronously stretching the primary hydrogel by adopting a winding device until the size is uniform, and forming after the primary hydrogel forms a stable structure to obtain the nanocomposite hydrogel optical fiber.
The preferred mode of the above preparation method is as follows:
the solvent in the step (1) is a mixed solution of water and glycerol, namely a two-component solvent; wherein the volume ratio of the glycerol to the water is 1:10-1: 1.
The inorganic cross-linking agent in the step (1) is one or two of lithium bentonite Laponite and silicon dioxide; the high light transmittance monomer is acrylamide AAm and oligoethylene glycol methyl ether methacrylate OEGMA, and the molar ratio of the high light transmittance monomer to the oligoethylene glycol methyl ether methacrylate OEGMA is defined as (M)AAm:MOEGMA0.1: 9.9-9.9: 0.1); the initiator is one or more of potassium persulfate, ammonium persulfate and sodium persulfate.
The molecular weight Mn of the oligomeric ethylene glycol methyl ether methacrylate OEGMA is 300-2000, wherein the molecular weight of the monomer OEGMA is adjustable.
The inorganic cross-linking agent in the step (1) accounts for 3-16 wt.% of the solvent content; the high light transmission monomer accounts for 10-30 wt.% of the mass of the solvent; the initiator is 1-10 wt.% of the mass of the monomers.
The accelerator in the step (2) is one of N, N, N ', N' -tetramethyl ethylenediamine and N, N-dimethylaniline, and the dosage of the accelerator is 0.2-0.8% of the volume of the pre-polymerization solution.
And (3) after an accelerator is added into the gel pre-polymerization liquid in the step (2), transferring the gel pre-polymerization liquid into a reaction tube within 1min for pre-polymerization reaction.
The reaction tube in the step (2) is a polytetrafluoroethylene tube, wherein the inner diameter of the tube is 1-3mm, and the length of the tube is 5-30 cm; the winding linear speed of the winding device is 2-12 m/min.
The diameter of the nano-composite hydrogel optical fiber in the step (2) is 100-1000 μm.
The invention relates to a nano-composite hydrogel optical fiber prepared by the method.
The invention provides an application of the nano composite hydrogel optical fiber.
Advantageous effects
(1) The preparation method adopts a polymerization-stretching synchronous method, and the internal network structure of the gel is changed from loose and porous to compact and stacked in the stretching and orientation process of the nascent hydrogel fiber which does not completely form a network, so that the mechanical strength of the nascent hydrogel fiber is improved, and the refractive index and the light guide performance of the nascent hydrogel fiber are effectively improved. Meanwhile, glycerin with lower hydrogen bonds is introduced into a water system, so that the volatility and the freezing temperature of the solvent are effectively reduced, the moisture retention of the prepared material is improved, and the use environment of the material is further widened; the invention has the advantages of easily obtained raw materials, simple process, remarkable performance improvement and great industrial production potential;
(2) the high-light-guiding and high-moisture-preserving nano composite hydrogel optical fiber prepared by the method is a hydrogel optical fiber with a high-orientation structure obtained by in-situ free radical polymerization and synchronous polymerization-stretching, has high mechanical strength, good light guiding performance and durable durability, and is expected to be applied to biosensing devices in various environments;
(3) the inorganic crosslinking points are all common materials sold in the market, so that the inorganic crosslinking agent is low in price and rich in storage;
(4) compared with the prior similar hydrogel optical fiber preparation technology, the method adopts in-situ polymerization and synchronous stretch spinning of monomers, gets rid of the technical problem of dissolution of high polymer, and has the advantages of simple process, no need of special equipment and easy industrial implementation.
Drawings
FIG. 1 is the IR spectrum of a high-light-guiding and high-moisture-retaining nanocomposite hydrogel optical fiber of Laponite/(AAm-co-OEGMA) in example 1;
FIG. 2 is a photo of a high-light-guiding and high-moisture-retaining nanocomposite hydrogel optical fiber material object of Laponite/(AAm-co-OEGMA) in example 1
FIG. 3 is an electron microscope photograph of the Laponite/(AAm-co-OEGMA) high-light-guiding and high-moisture-retaining nanocomposite hydrogel fiber optic fiber in example 1;
FIG. 4 is a graph showing the optical loss performance of the Laponite/(AAm-co-OEGMA) high-light-guiding and high-moisture-retaining nanocomposite hydrogel optical fiber in example 1;
FIG. 5 is a graph of the moisturizing ratio of the Laponite/(AAm-co-OEGMA) highly light-conductive and highly moisturizing nanocomposite hydrogel optical fiber in example 1.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
The required materials are as follows: oligoethylene glycol methyl ether methacrylate OEGMA (Mn ═ 300/500/2000), acrylamide AAm (Mw ═ 71), N-tetramethylethylenediamine (Mw ═ 116.2), N-dimethylaniline (Mw ═ 121.18) were supplied from Sigma-Aldrich co., ltd., potassium persulfate (Mw ═ 270.32), ammonium persulfate (Mw ═ 228.2), and glycerin (glycerol f.w.: 92.09) were supplied from the national group chemicals co., ltd., and Laponite (monolithic layer thickness-1 nm, diameter-25 nm), and silica (particle size 20nm D50) were supplied from BYK Additives & Instruments. All materials were used without further purification. Deionized water was prepared by a NW ultra-pure water system from Heal Force.
The test method comprises the following steps:
1. testing the performance of the light guide: the transmission loss of various hydrogel fibers is measured by a cutback method, and a 532-nanometer laser is coupled with a hydrogel optical fiber. The power of light passing through the hydrogel optical fiber is measured by a power meter, the tail end of the optical fiber is cut off by 1cm by a sharp knife, the output power is measured, the measurement is repeated every 1cm, 7 points are measured, and the loss value is calculated.
2. And (3) testing the moisture retention rate: and (3) placing the hydrogel fiber which reaches the swelling balance in an environment with the temperature of 25 ℃ and the RH of 20 percent, measuring the mass of the hydrogel fiber every 1 hour, and obtaining the moisture retention rate of the hydrogel by the ratio of the measured value to the mass at the initial balance.
3. The tensile property test method comprises the following steps: the tensile property of the prepared hydrogel fiber is tested by an Instron instrument under the environment of 23 ℃ and 60% RH, the distance between clamps is 100mm, the tensile speed is 100mm/min, the number of times of the sample is 5, the diameter of the fiber is input before the tensile test for the instrument to calculate the tensile strength (the diameter is calculated by observing through a microscope), and the tensile test is carried out by giving a tensile program to obtain the tensile strength and the elongation at break of the sample.
Example 1
8g of deionized water, 2g of glycerol, 1.4g of lithium bentonite Laponite, 0.03g of potassium persulfate, 0.6g of oligoethylene glycol monomethyl ether methacrylate (Mn 500) and 1.4g of acrylamide monomer were weighed at room temperature and stirred for 5 hours until the potassium persulfate was completely dissolved to obtain a gel prepolymer. mu.L of accelerator N, N, N, N-tetramethylethylenediamine was added to the gel prepolymer solution, and the prepolymer solution was rapidly transferred to a polytetrafluoroethylene tube having an inner diameter of 2mm and a length of 30cm within 1 minute. After the reaction is carried out for 5 minutes, the nascent hydrogel fiber is extruded through a 40mL needle tube, meanwhile, the nascent hydrogel fiber is wound and collected at a position 50cm away from the opening of a polytetrafluoroethylene tube, the linear speed of a winding roller is 12m/min, and the nano composite hydrogel optical fiber with the diameter of about 250 micrometers is obtained after the forming of the nascent hydrogel fiber is completed, the refractive index of the prepared nano composite hydrogel optical fiber measured through a refractometer is 1.79 due to the compact structure inside the nano composite hydrogel optical fiber, and the refractive index is greatly improved compared with that of nano composite hydrogel (the refractive index is 1.45) with the same components. And then testing the tensile property of the nano composite hydrogel optical fiber by an Instron, wherein the tensile strength of the nano composite hydrogel optical fiber is 4.7MPa, and the elongation at break is 194 percent.
Laponite/(AAm-co-OEGMA) high-light guiding and high-securityThe wet nanocomposite hydrogel fiber optic infrared spectrum is shown in figure 1. As can be seen from the figure, the thickness of the nanocomposite hydrogel optical fiber is also 1001cm-1That is, an absorption peak appears at an absorption peak of the Laponite, but no obvious characteristic absorption peak exists in the monomer, which shows that the method can well compound the two monomers and the Laponite to prepare the Laponite/(AAm-co-OEGMA) nano composite hydrogel optical fiber.
A Laponite/(AAm-co-OEGMA) high-light-guiding and high-moisture-retention nanocomposite hydrogel optical fiber physical photograph is shown in FIG. 2. As can be seen from the figure, the nano-composite hydrogel optical fiber prepared by the method has good photoconductive performance and flexibility.
A high-light-guiding and high-moisture-keeping nanocomposite hydrogel fiber optic electron microscope photograph of Lamonite/(AAm-co-OEGMA) is shown in FIG. 3. The nano composite hydrogel optical fiber prepared by the method has a continuous structure and uniform appearance.
The graph of the optical loss performance of the Laponite/(AAm-co-OEGMA) high-light-guiding and high-moisture-retaining nanocomposite hydrogel optical fiber is shown in FIG. 4. As can be seen from the figure, the optical loss per centimeter of the nano-composite hydrogel optical fiber prepared by the method is only 0.3dB, the optical guide performance is superior to 0.45dB/cm of the alginic acid/polyacrylamide hybrid hydrogel optical fiber prepared by professor Seok-Hyun Yun of Harvard medical institute, and the Laponite/(AAm-co-OEGMA) hydrogel optical fiber prepared by using a template method through similar monomers as the monomer in the invention in the figure 4, and the preparation method is as follows: 10g of deionized water, 1.4g of lithium bentonite Laponite, 0.03g of potassium persulfate, 0.6g of oligoethylene glycol methyl ether methacrylate (Mn ═ 500) and 1.4g of acrylamide monomer were fed into a polytetrafluoroethylene tube having a diameter of 300. mu.m, and the tube was heated to 80 ℃ to initiate radical polymerization in situ, and after 12 hours of molding, the tube was removed from the tube, and the light conductivity thereof was about 1.6dB/cm as measured by the cutback method.
The graph of the moisture retention rate of the Laponite/(AAm-co-OEGMA) high-light-guiding and high-moisture-retaining nanocomposite hydrogel optical fiber is shown in FIG. 5. As can be seen from the figure, the moisture retention rate of the nano composite hydrogel optical fiber prepared by the method after reaching the swelling equilibrium for 480 hours at 25 ℃ and 20% relative humidity is more than twice of that of a similar self-made hydrogel material, wherein the moisture retention rate is 70%.
(the home-made similar hydrogel material is specifically that a prepolymerization solution prepared from 10g of deionized water, 1.4g of Laponite, 0.03g of potassium persulfate, 0.6g of oligoethylene glycol methyl ether methacrylate (Mn ═ 500) and 1.4g of acrylamide monomer is introduced into a polytetrafluoroethylene tube with the diameter of 300 mu m, the temperature is increased to 80 ℃ to initiate in-situ free radical polymerization, the gel is taken out of the tube after being formed for 12 hours, and the moisture retention rate of the gel is tested).
Example 2
6g of deionized water, 4g of glycerol, 1g of lithium bentonite Laponite, 0.04g of ammonium persulfate, 1g of oligoethylene glycol methyl ether methacrylate (Mn 300) and 1g of acrylamide monomer are weighed at room temperature and stirred for 6 hours until potassium persulfate is completely dissolved to obtain a gel pre-polymerization solution. mu.L of accelerator N, N, N, N-tetramethylethylenediamine was added to the gel prepolymer solution, and the prepolymer solution was rapidly transferred to a polytetrafluoroethylene tube of 3mm inner diameter and 20cm length within 30 seconds. After reacting for 3 minutes, extruding out the primary hydrogel fiber through a 40mL needle tube, simultaneously winding and collecting at a position 20cm away from the polytetrafluoroethylene tube opening, wherein the linear speed of a winding roller is 8m/min, and obtaining the nano-composite hydrogel optical fiber with the diameter of about 300 mu m after the molding is finished, wherein the refractive index of the prepared nano-composite hydrogel optical fiber measured through a refractometer is 1.59, which is greatly improved compared with the nano-composite hydrogel (the refractive index is 1.39) with the same components. And then testing the tensile property of the nano composite hydrogel optical fiber by an Instron, wherein the tensile strength of the nano composite hydrogel optical fiber is-2.8 MPa, and the elongation at break is-323%.
Example 3
3g of deionized water, 2g of glycerol, 0.25g of silica, 0.03g of potassium persulfate, 0.4g of OEGMA (Mn 2000) and 0.6g of acrylamide monomer were weighed at room temperature and stirred for 5 hours until the potassium persulfate was completely dissolved to obtain a gel prepolymer. mu.L of accelerator N, N-dimethylaniline was added to the gel prepolymer solution and the prepolymer solution was rapidly transferred to a 25cm long polytetrafluoroethylene tube having an internal diameter of 1mm within 1 minute. After reacting for 12 minutes, extruding the nascent hydrogel fiber through a 20mL needle tube, simultaneously winding and collecting at a position 10cm away from the polytetrafluoroethylene tube opening, wherein the linear speed of a winding roller is 6m/min, and obtaining the nano-composite hydrogel optical fiber with the diameter of about 100 mu m after the molding is finished, wherein the refractive index of the prepared nano-composite hydrogel optical fiber measured by a refractometer is 1.74, which is greatly improved compared with the nano-composite hydrogel (the refractive index is 1.42) with the same components. And then testing the tensile property of the nano composite hydrogel optical fiber by an Instron, wherein the tensile strength of the nano composite hydrogel optical fiber is-3.4 MPa, and the elongation at break is-248 percent.
Claims (10)
1. A nanocomposite hydrogel optical fiber, wherein the optical fiber is obtained by in-situ polymerization and simultaneous stretching of a system comprising the following components; wherein the system components comprise: a mixture of water and glycerol, an inorganic cross-linking agent, a high light transmittance monomer and an initiator; wherein the high light transmittance monomer is acrylamide AAm and oligoethylene glycol methyl ether methacrylate OEGMA, the inorganic cross-linking agent is lithium bentonite Laponite and/or silicon dioxide, and the system also comprises an accelerator.
2. The optical fiber of claim 1, wherein the glycerol to water volume ratio is 1:10 to 1: 1; the initiator is one or more of potassium persulfate, ammonium persulfate and sodium persulfate.
3. A method for preparing a nanocomposite hydrogel optical fiber, comprising:
(1) uniformly mixing an inorganic cross-linking agent, a solvent, a high-light-transmittance monomer and an initiator to obtain a gel pre-polymerization solution; wherein the inorganic cross-linking agent is lithium bentonite Laponite and/or silicon dioxide; the high light-transmitting monomer is acrylamide AAm and oligoethylene glycol methyl ether methacrylate OEGMA;
(2) and adding an accelerator into the gel prepolymerization solution, transferring the gel prepolymerization solution into a reaction tube for prepolymerization reaction, extruding the primary hydrogel in the reaction tube after the reaction is carried out for 3-20min, synchronously stretching the primary hydrogel by adopting a winding device, and forming to obtain the nanocomposite hydrogel optical fiber.
4. The preparation method according to claim 3, wherein the solvent in the step (1) is a mixed solution of water and glycerin; wherein the volume ratio of the glycerol to the water is 1:10-1: 1.
5. The preparation method according to claim 3, wherein the initiator in the step (1) is one or more of potassium persulfate, ammonium persulfate and sodium persulfate; the inorganic cross-linking agent is 3-16 wt.% of the mass of the solvent; the high light transmission monomer accounts for 10-30 wt.% of the mass of the solvent; the initiator is 1-10 wt.% of the mass of the monomers.
6. The method according to claim 3, wherein the accelerator in step (2) is one of N, N, N ', N' -tetramethylethylenediamine and N, N-dimethylaniline, and the amount of the accelerator is 0.2-0.8% by volume of the prepolymer solution.
7. The process according to claim 3, wherein the reaction tube in the step (2) is a polytetrafluoroethylene tube, wherein the tube has an inner diameter of 1 to 3mm and a length of 5 to 30 cm; the winding linear speed of the winding device is 2-12 m/min.
8. The method as claimed in claim 3, wherein the diameter of the nanocomposite hydrogel optical fiber in the step (2) is 100-1000 μm.
9. A nanocomposite hydrogel optical fiber prepared by the method of claim 3.
10. Use of the nanocomposite hydrogel optical fiber of claim 1 in a biosensing device.
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| CN110923838A (en) | 2020-03-27 |
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