CN1140547C - Process for preparing nano SiO2 modified optical plastic fibres - Google Patents
Process for preparing nano SiO2 modified optical plastic fibres Download PDFInfo
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- CN1140547C CN1140547C CNB011153113A CN01115311A CN1140547C CN 1140547 C CN1140547 C CN 1140547C CN B011153113 A CNB011153113 A CN B011153113A CN 01115311 A CN01115311 A CN 01115311A CN 1140547 C CN1140547 C CN 1140547C
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Abstract
The present invention belongs to the technical field of nanometer material and plastic optical fibers, which particularly relates to a method for preparing nanometer silicon dioxide modified plastic optical fibers. Mixed solution of methacrylic ester monomers and siloxane compounds is taken according to the weight ratio of 5: 1 to 50: 1, and azo or peroxide initiating agents accounting for 0.1% to 1% of the total weight of the mixed solution and thiol chain transfer agents accounting for 0.03% to 0.2% of the total weight of the mixed solution are added. The mixed solution is heated, and a plastic optical fiber prepolymerized rod is drawn into a plastic optical fiber. The prepared plastic optical fiber is soaked into mixed solution of ammonia water and alcohol, and SiO2 nanometer particles are formed by swelling and chemical reaction. The plastic optical fiber is extracted from soak solution, and ammonia water and alcohol are volatilized thoroughly. The mechanical properties and the optical properties of the obtained nanometer SiO2 modified plastic optical fiber are enhanced.
Description
The invention belongs to the technical field of nano materials and plastic optical fibers, and particularly relates to a method for preparing a nano silicon dioxide modified plastic optical fiber.
The plastic optical fiber has the characteristics of large fiber core diameter, easy processing, good flexibility, easy installation and maintenance and low cost, and the bandwidth of the plastic optical fiber is hundreds of times higher than that of the traditional copper stranded wire medium, so that the plastic optical fiber is the first-choice transmission medium for local area networks and optical fibers to enter homes, and various high-performance plastic optical fibers are rapidly developed in recent years.
The prior nanotechnology provides a brand-new method for preparing novel materials, wherein the application of inorganic nanometer components for modifying high molecular polymers is widely reported; the modified polymer material has excellent optical property, mechanical property and chemical property, reduces the phase separation degree of inorganic components and polymer components along with the development of theoretical research and preparation technology, and has wide application prospect.
The invention aims to provide a method for preparing a nano silicon dioxide modified plastic optical fiber, which does not need to change the traditional equipment for preparing the plastic optical fiber, and is simple and easy to operate.
It is another object of the present invention to provide a modified plastic optical fiber having dual characteristics of an inorganic silica optical fiber and a plastic optical fiber, which can improve the flexural resistance, impact resistance and heat resistance of the plastic optical fiber: the method has the characteristics of low signal transmission loss and low product cost.
The technical scheme of the invention is to apply the nanotechnology to the preparation of the plastic optical fiber.
(1) Mixing siloxane compounds in methacrylate monomers, adding an initiator and a thiol chain transfer agent, and heating and polymerizing to obtain a plastic optical fiber pre-polymerization rod;
(2) heating, and drawing the plastic optical fiber pre-polymerization rod into a plastic optical fiber with a required diameter;
(3) immersing the prepared plastic optical fiber into a mixed solution of ammonia and alcohol, wherein the alcohol gradually swells the plastic optical fiber, and simultaneously, water and alcohol are mixed under alkaline conditionsReacting the siloxane compound until the reaction is complete; formation of SiO2Nanoparticles, the reaction formula is as follows:
wherein: r represents methyl, ethyl, propyl, gamma-aminopropyl or the like.
Because the reaction is carried out among solid polymer chains, the nano particles are stabilized and protected; is not easy to aggregate; meanwhile, because the radial distance of the plastic optical fiber is short, swelling and chemical reaction can be completed quickly, and the particle size distribution of the nano particles is uniform and consistent.
(4) And taking out the plastic optical fiber from the soaking solution to completely volatilize alcohol and ammonia water, thereby preparing the nano silicon dioxide modified plastic optical fiber.
The specific method for preparing the nano silicon dioxide modified plastic optical fiber comprises the following steps:
(1) taking methacrylate monomers and siloxane compounds, wherein the methacrylate monomers comprise: the weight ratio of the siloxane compounds is 5: 1-50: 1, and mixed liquid is prepared; adding azo or peroxide initiator in 0.1-1 wt% and mercaptan chain transfer agent in 0.03-0.2 wt% into the mixture, and heating to polymerize to obtain pre-polymerized plastic fiber rod.
(2) And drawing the pre-polymer rod of the plastic optical fiber into the plastic optical fiber with a certain diameter on a fiber drawing machine.
(3) Soaking the prepared plastic optical fiber into a mixed solution of 25 wt% ammonia water and alcohol for swelling, and reacting in a high polymer material to generate SiO2Nano particles, wherein the weight ratio of ammonia water to alcohol is 1: 10-1: 100.
(4) Taking the plastic optical fiber prepared in the step (3), and completely volatilizing alcohol and a small amount of ammonia water in the plastic optical fiber under the normal pressure or reduced pressure condition to prepare the nano silicon dioxide modified plastic optical fiber.
The methacrylate monomer is methyl methacrylate, ethyl methacrylate, phenyl methacrylate or the like; the siloxane compound is tetramethyl orthosilicate, tetraethyl orthosilicate or gamma-aminopropyltriethoxysilane, etc.; the alcohol is methanol, ethanol, propanol or isopropanol; the initiator is azobisisobutyronitrile or benzoyl peroxide and the like; the chain transfer agent is n-butyl mercaptan, dodecyl mercaptan, hexadecyl mercaptan, etc.
The nanometer SiO prepared by the invention2The modified plastic optical fiber has the characteristics of low loss, high hardness, good aging resistance, strong flexibility resistance, high temperature resistance and the like; and the equipment is simple, the method is easy to implement, and the reaction condition is mild.
The nanometer SiO prepared by the invention2The modified plastic optical fiber improves the photoelectric property, the thermal property and the mechanical property of the traditional plastic optical fiber, and can be applied to network information communication, display systems, sensing devices, instrument illumination and other aspects.
The nano silicon dioxide modified plastic optical fiber prepared by the invention has the dual characteristics of inorganic quartz optical fiber and plastic optical fiber; the mechanical property of the plastic optical fiber can be improved, and the flexibility resistance, the impact resistance, the hardness and the like are obviously enhanced; the optical performance of the plastic optical fiber can be improved, so that the transmission loss of optical fiber signals is reduced; various physical and chemical properties are improved, and particularly, the aging resistance and the temperature resistance are obviously improved.
The technical solution of the present invention is further described below with reference to the following examples:
example 1
Taking methyl methacrylate and tetraethyl orthosilicate with the weight ratio of 20: 1 to prepare a mixed solution, adding azobisisobutyronitrile and 0.03% of n-butyl mercaptan which account for 0.1% of the total weight of the mixed solution, and heating and polymerizing to form the plastic optical fiber pre-polymerization rod. The obtained plastic optical fiber pre-polymerization rod is thermally drawn into a plastic optical fiber with a certain diameter on a fiber drawing machine, then the plastic optical fiber is immersed into a mixed solution of ammonia water and methanol with the weight percentage concentration of 25 percent for swelling and reaction till the completion, and SiO is generated in the plastic optical fiber through the reaction2Nano particles, wherein the weight ratio of ammonia water to methanol is 1: 20. Taking out the plastic optical fiber, and volatilizing methanol and ammonia water from the optical fiber under normal pressure to prepare the sodiumRice silica modified plastic optical fiber.
Example 2
Taking methyl methacrylate and tetramethyl orthosilicate with the weight ratio of methyl methacrylate to tetramethyl orthosilicate being 20: 1, preparing a mixed solution, adding azodiisobutyronitrile and n-butyl mercaptan which account for 0.3 percent of the total weight of the mixed solution, and heating and polymerizing to obtain the plastic optical fiber pre-polymerization rod. The obtained plastic optical fiber pre-polymerization rod is hot-drawn into a plastic optical fiber with a certain diameter on a fiber drawing machine, then the plastic optical fiber is immersed into a mixed solution of 25 percent ammonia water and ethanol for swelling, and the mixture reacts in the plastic optical fiber to generate SiO2Nano particles, wherein the weight ratio of ammonia water to ethanol is 1: 40. The plastic optical fiber was taken out, and ethanol and ammonia were completely volatilized from the optical fiber under reduced pressure to prepare a nano-silica modified plastic optical fiber.
Example 3
Taking methyl methacrylate and tetraethyl orthosilicate in a weight ratio of 20: 1 to prepare a mixed solution, and adding azobisisobutyronitrile accounting for 1 percent of the total weight of the mixed solution and 0.1 percent of n-butyl mercaptan. Heating and polymerizing the solution to obtain the plastic optical fiber pre-polymerization rod. The obtained plastic optical fiber pre-polymerization rod is thermally drawn into a plastic optical fiber with a certain diameter on a fiber drawing machine, then the plastic optical fiber is immersed into a mixed solution of 25 percent ammonia water and isopropanol for swelling and reaction till the completion, and SiO is generated in the plastic optical fiber through reaction2Nano particles, wherein the weight ratio of ammonia water to isopropanol is 1: 20. The plastic optical fiber was taken out, and isopropanol and ammonia water were completely volatilized from the optical fiber under reduced pressure to prepare a nano-silica modified plastic optical fiber.
Example 4
Taking methyl methacrylate and tetraethyl orthosilicate with the weight ratio of 50: 1 to prepare a mixed solution, and adding azobisisobutyronitrile accounting for 0.1 percent of the total weight of the mixed solution and 0.05 percent of the mixed solutionN-butyl mercaptan. The obtained plastic optical fiber pre-polymerization rod is hot-drawn into a plastic optical fiber with a certain diameter on a fiber drawing machine, and then the plastic optical fiber is immersed into a mixed solution of 25 percent ammonia water and methanol for swelling and reactionTo complete, the reaction generates SiO in the plastic optical fiber2Nano particles, wherein the weight ratio of ammonia water to methanol is 1: 100. And taking out the plastic optical fiber, and completely volatilizing the methanol and the ammonia water from the optical fiber under normal pressure to prepare the nano silicon dioxide modified plastic optical fiber.
Example 5
Taking methyl methacrylate and tetraethyl orthosilicate in a weight ratio of 40: 1 to prepare a mixed solution, and adding benzoyl peroxide and dodecyl mercaptan in an amount which is 1 percent of the total weight of the mixed solution and 0.08 percent of the total weight of the mixed solution. Heating and polymerizing the solution to obtain the plastic optical fiber pre-polymerization rod. The obtained plastic optical fiber pre-polymerization rod is thermally drawn into a plastic optical fiber with a certain diameter on a fiber drawing machine, then the plastic optical fiber is immersed into a mixed solution of ammonia water and methanol with the concentration of 25 percent for swelling and reaction till the completion, and SiO is generated by the reaction in the plastic optical fiber2Nano particles, wherein the weight ratio of ammonia water to methanol is 1: 10. And taking out the plastic optical fiber, and completely volatilizing the methanol and the ammonia water from the optical fiber under normal pressure to prepare the nano silicon dioxide modified plastic optical fiber.
Example 6
Taking phenyl methacrylate and gamma-aminopropyltriethoxysilane, wherein the weight ratio of the phenyl methacrylate to the gamma-aminopropyltriethoxysilane is 40: 1, preparing a mixed solution, and adding azobisisobutyronitrile accounting for 0.1 percent of the total weight of the mixed solution and 0.03 percent of n-butyl mercaptan into the mixed solution. The obtained plastic optical fiber pre-polymerization rod is thermally drawn into a plastic optical fiber with a certain diameter on a fiber drawing machine, then the plastic optical fiber is immersed into a mixed solution of ammonia water and methanol with the concentration of 25 percent for swelling and reaction till the completion, and SiO is generated by the reaction in the plastic optical fiber2Nano particles, wherein the weight ratio of ammonia water to methanol is 1: 60. The plastic optical fiber was taken out, and methanol and ammonia were completely volatilized from the optical fiber under reduced pressure to prepare a nano-silica modified plastic optical fiber.
Example 7
Taking ethyl methacrylate and tetraethyl orthosilicate with the weight ratio of 30: 1 to prepare a mixed solution, and adding azobisisobutyronitrile accounting for 0.1 percent of the total weight of the mixed solution and n-butyl accounting for 0.03 percent of the total weight of the mixed solutionA thiol group. The obtained plastic optical fiber pre-polymerization rod is thermally drawn into a plastic optical fiber with a certain diameter on a fiber drawing machine, then the plastic optical fiber is immersed into a mixed solution of 25 percent ammonia water and ethanol for swelling and reaction till the completion, and the plastic optical fiber is reacted in the plastic optical fiber to generate SiO2Nano particles, wherein the weight ratio of ammonia water to ethanol is 1: 60. The plastic optical fiber was taken out, and ethanol and ammonia were completely volatilized from the optical fiber under reduced pressure to prepare a nano-silica modified plastic optical fiber.
Example 8
Taking methyl methacrylate and tetramethyl orthosilicate with the weight ratio of methyl methacrylate to tetramethyl orthosilicate being 20: 1, preparing a mixed solution, adding benzoyl peroxide and n-butyl mercaptan which account for 0.3 percent of the total weight of the mixed solution and 0.05 percent of the total weight of the mixed solution, and heating and polymerizing to form the plastic optical fiber pre-polymerization rod. The obtained plastic optical fiber pre-polymerization rod is thermally drawn into a plastic optical fiber with a certain diameter on a fiber drawing machine, then the plastic optical fiber is immersed into a mixed solution of 25 percent ammonia water and isopropanol for swelling, and the mixture reacts in the plastic optical fiber to generate SiO2Nano particles, wherein the weight ratio of ammonia water to isopropanol is 1: 40. The plastic optical fiber was taken out, and isopropanol and ammonia water were completely volatilized from the optical fiber under reduced pressure to prepare a nano-silica modified plastic optical fiber.
Claims (6)
1. A method for preparing a nano-silica modified plastic optical fiber is characterized by comprising the following steps: the method comprises the following steps:
(1) mixing siloxane compounds in methacrylate monomers to prepare a mixed solution; adding an initiator and a mercaptan chain transfer agent, and heating and polymerizing to obtain a plastic optical fiber pre-polymerization rod; wherein, methacrylate monomer: the weight ratio of the siloxane compound is 5: 1-50: 1, the adding amount of the azo or peroxide initiator accounts for 0.1-1% of the total weight of the mixed solution, and the mercaptan chain transfer agent accounts for 0.03-0.2%;
(2) heating, and drawing the plastic optical fiber pre-polymerization rod into a plastic optical fiber with a required diameter;
(3) the ammonia water and the alcohol are mixed together,obtaining mixed solution of ammonia water and alcohol, wherein the weight ratio of the ammonia water to the alcohol is 1: 10-1: 100, and the concentration of the ammonia water is 25%; immersing the prepared plastic optical fiber into a mixed solution of ammonia water and alcohol, wherein the alcohol gradually swells the plastic optical fiber, and simultaneously, water and siloxane compounds react under an alkaline condition until the reaction is complete to form SiO2A nanoparticle;
(4) and taking out the plastic optical fiber from the soaking solution to completely volatilize alcohol and ammonia water, thereby preparing the nano silicon dioxide modified plastic optical fiber.
2. The method of claim 1, wherein: the methacrylate monomer is methyl methacrylate, ethyl methacrylate or phenyl methacrylate.
3. The method of claim 1, wherein: the siloxane compound is tetramethyl orthosilicate, tetraethyl orthosilicate or gamma-aminopropyltriethoxysilane.
4. The method of claim 1, wherein: the initiator is azobisisobutyronitrile or benzoyl peroxide.
5. The method of claim 1, wherein: the chain transfer agent is n-butyl mercaptan, dodecyl mercaptan or hexadecyl mercaptan.
6. The method of claim 1, wherein: the alcohol is methanol, ethanol, propanol or isopropanol.
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| CNB011153113A CN1140547C (en) | 2001-04-18 | 2001-04-18 | Process for preparing nano SiO2 modified optical plastic fibres |
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| CNB011153113A CN1140547C (en) | 2001-04-18 | 2001-04-18 | Process for preparing nano SiO2 modified optical plastic fibres |
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| CN1140547C true CN1140547C (en) | 2004-03-03 |
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| CN116832584A (en) * | 2023-08-02 | 2023-10-03 | 山东绿知源环保工程有限公司 | Waste gas collecting and purifying device for desulfurization workshop of coking plant |
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