CN111592769A - OPGW hydrogen absorption optical fiber filling paste and production process thereof - Google Patents

OPGW hydrogen absorption optical fiber filling paste and production process thereof Download PDF

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CN111592769A
CN111592769A CN202010307309.0A CN202010307309A CN111592769A CN 111592769 A CN111592769 A CN 111592769A CN 202010307309 A CN202010307309 A CN 202010307309A CN 111592769 A CN111592769 A CN 111592769A
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optical fiber
hydrogen
molecular sieve
opgw
hydrogen absorption
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蓝云燕
何承平
黄燕生
黄建生
廖连英
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Shenzhen Mpd Hitech Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L91/00Compositions of oils, fats or waxes; Compositions of derivatives thereof
    • C08L91/06Waxes
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B6/00Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
    • G02B6/44Mechanical structures for providing tensile strength and external protection for fibres, e.g. optical transmission cables
    • G02B6/4401Optical cables
    • G02B6/4429Means specially adapted for strengthening or protecting the cables
    • G02B6/44382Means specially adapted for strengthening or protecting the cables the means comprising hydrogen absorbing materials
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B6/00Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
    • G02B6/44Mechanical structures for providing tensile strength and external protection for fibres, e.g. optical transmission cables
    • G02B6/4479Manufacturing methods of optical cables
    • G02B6/4483Injection or filling devices
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/005Additives being defined by their particle size in general
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/006Additives being defined by their surface area
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend

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  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Surface Treatment Of Glass Fibres Or Filaments (AREA)

Abstract

The invention discloses an OPGW hydrogen absorption optical fiber filling paste and a production process thereof, relating to the technical field of OPGW optical cable construction; an OPGW hydrogen absorption optical fiber filling paste is mainly prepared from the following filling paste raw materials in parts by weight: 80-90 parts of base oil, 3-15 parts of organic thickening agent, 0.1-1 part of antioxidant, 0.1-1 part of dispersion stabilizer, 0.1-2 parts of pour point depressant and 0.1-5 parts of hydrogen absorption material, wherein the hydrogen absorption material is a silver molecular sieve; the optical fiber transmission device has the advantages of improving the optical fiber transmission quality to a certain extent and being low in cost; the production process of the OPGW hydrogen absorption optical fiber filling paste comprises the following steps: degassing, mixing and dissolving, dispersing, hydrogen absorption treatment, air extraction and the like; the production process of the OPGW hydrogen absorption optical fiber filling paste has the advantage of improving the product compatibility conveniently.

Description

OPGW hydrogen absorption optical fiber filling paste and production process thereof
Technical Field
The invention relates to the technical field of preparation of optical fiber filling paste, in particular to OPGW hydrogen absorption optical fiber filling paste and a production process thereof.
Background
The OPGW optical cable, also called optical fiber composite overhead ground wire, is used for placing optical fibers in the ground wire of an overhead high-voltage transmission line to form an optical fiber communication network on the transmission line, and the structural form has the double functions of the ground wire and communication. Because the optical fiber in the OPGW optical cable has the characteristics of electromagnetic interference resistance, light dead weight and the like, the OPGW optical cable can be arranged at the top of a power transmission line tower without considering the problems of optimal hanging position, electromagnetic corrosion and the like. Therefore, the OPGW has the obvious characteristics of higher reliability, superior mechanical performance, lower cost and the like, and has wide application in the field of optical cables.
In order to protect the optical fiber, it is often necessary to fill the optical fiber casing with an optical fiber filling paste, which can prevent moisture or moisture in the air from corroding the optical fiber on one hand, and play a role of a cushion for the optical fiber on the other hand, so as to buffer the optical fiber from being affected by mechanical forces such as vibration, impact, bending, and the like, and play a role of protecting the optical fiber. The metal parts in the optical cable can emit hydrogen in the corrosion process and the stainless steel optical cable sleeve welding process, and the hydrogen can cause the attenuation of optical fiber transmission signals to be increased, so that the transmission performance is obviously reduced, therefore, a hydrogen absorbing material needs to be added into the optical fiber filling paste to reduce the influence of the hydrogen on the optical fiber signals.
Application publication No. CN102778735A discloses a hydrogen-absorbing fiber paste for OPGW optical cables and a manufacturing method thereof, which comprises 75-85% of base oil, 6-10% of gelling agent, 0.3-0.6% of antioxidant, 0.8-1% of viscosity index improver, 1.5-2% of oil separation inhibitor and 2-5% of hydrogen-absorbing agent in percentage by weight. According to the technical scheme, palladium (Pd) is dispersed on an active carbon carrier to form a catalyst, and then the catalyst is mixed with an organic hydrogen absorption component 1, 4 bis (phenylethynyl) benzene (DEB) to prepare the hydrogen absorption agent. According to the technical scheme, the hydrogen absorption agent containing the activated carbon with high specific surface area, the noble metal palladium and the 1, 4 bis (phenylethynyl) benzene (DEB) is added, so that the hydrogen absorption performance of the hydrogen absorption fiber paste is improved, the incompatibility of the fiber paste and stainless steel and hydrogen generated in a welding process are eliminated, the defects in an optical fiber lattice are reduced, the loss of the optical fiber is reduced, and the transmission performance of the optical fiber is improved.
However, this solution has the following drawbacks: 1. expensive noble metal palladium is used, so that the preparation cost of the hydrogen absorption fiber paste is increased, and the market competitiveness of the product is reduced; 2. the hydrogen absorbing agent carrier used in the technical scheme is activated carbon with high specific surface area, the activated carbon material has poor adhesion and high hardness, and the activated carbon material and other raw materials in the hydrogen absorbing fiber paste have poor compatibility, so that the protection effect of the product on the optical fiber can be influenced, and certain adverse effect is brought to the transmission quality of the optical fiber.
Disclosure of Invention
In view of the defects of the prior art, the first object of the present invention is to provide a filling paste for OPGW hydrogen absorption optical fiber, which can improve the optical fiber transmission quality to some extent, and has the advantages of improving the optical fiber transmission quality to some extent and low cost.
A second object of the present invention is to provide a process for producing an OPGW hydrogen-absorbing optical fiber filling paste that facilitates improving product compatibility, which has the advantage of facilitating improving product compatibility.
In order to achieve the first object, the invention provides the following technical scheme: an OPGW hydrogen absorption optical fiber filling paste is mainly prepared from the following filling paste raw materials in parts by weight: 80-90 parts of base oil, 3-15 parts of organic thickening agent, 0.1-1 part of antioxidant, 0.1-1 part of dispersion stabilizer, 0.1-2 parts of pour point depressant and 0.1-5 parts of hydrogen absorption material, wherein the hydrogen absorption material is a silver molecular sieve.
By adopting the technical scheme, the silver molecular sieve hydrogen absorption material is used, hydrogen is embedded in crystal lattices of the molecular sieve carrier in the using process, hydrogen atoms in the hydrogen are catalyzed by silver ions to react with oxygen elements in any form to form water which is stored in molecular sieve pore channels, the hydrogen concentration existing around the optical fiber is obviously reduced, and the adverse effect of the hydrogen in the optical cable on the transmission quality of the optical fiber can be obviously reduced; the silver molecular sieve hydrogen absorption material is used, the main component of the silver molecular sieve hydrogen absorption material is a molecular sieve, the main component of the molecular sieve is aluminosilicate, the aluminosilicate has strong adhesion force and better adhesion effect, has better compatibility with base oil, can be better bonded with the base oil, and avoids adverse effects brought by the use of active carbon on the compatibility of the hydrogen absorption fiber paste, so that adverse effects brought by the use of the active carbon on the viscosity and thixotropy of the hydrogen absorption fiber paste are avoided, and the transmission quality of the optical fiber is improved to a certain extent; the invention uses the silver molecular sieve hydrogen absorption material, avoids the use of expensive noble metal palladium, and reduces the production cost of the hydrogen absorption optical fiber filling paste.
Preferably, the filling paste is mainly prepared from the following filling paste raw materials in parts by weight: 80-90 parts of base oil, 5-15 parts of organic thickening agent, 0.3-0.8 part of antioxidant, 0.2-0.8 part of dispersion stabilizer, 0.5-1.5 parts of pour point depressant and 0.5-5 parts of silver molecular sieve
By adopting the technical scheme, the OPGW hydrogen-absorbing optical fiber filling paste with excellent compatibility, viscosity and thixotropic property is prepared by using a better raw material ratio, so that the transmission quality of optical fibers is improved, and the market competitiveness of products is improved.
Preferably, the silver molecular sieve is mainly prepared from the following hydrogen absorption raw materials in parts by weight: 0.4-4 parts of molecular sieve and 0.1-1 part of silver nitrate.
By adopting the technical scheme, in the using process, hydrogen is embedded in crystal lattices of the molecular sieve carrier, hydrogen atoms in the hydrogen are catalyzed by silver ions to react with oxygen elements in any form to form water which is stored in a molecular sieve pore channel, the silver ions and the molecular sieve are used as hydrogen absorption materials with proper proportion, the hydrogen concentration around the optical fiber is obviously reduced through the coordination effect of the molecular sieve and the silver ions, the adverse effect of the hydrogen in the optical cable on the transmission quality of the optical fiber can be obviously reduced, the transmission quality of the optical fiber is improved, and the market competitiveness of products is improved.
Preferably, the molecular sieve is an HY type molecular sieve, the specific surface area of the HY type molecular sieve is 600 square meters per gram to 800 square meters per gram, and the particle size of the HY type molecular sieve is 0.2 to 2 micrometers.
By adopting the technical scheme, the HY molecular sieve with high specific surface area is used, has larger pore volume and larger adsorption capacity for hydrogen, can convert more hydrogen under the coordination of silver ions, improves the hydrogen absorption performance of products, further reduces the hydrogen concentration around the optical fiber, improves the transmission quality of the optical fiber and improves the market competitiveness of the products; and the HY molecular sieve with small particle size has higher viscosity and stronger adsorption force, can be better bonded with base oil, improves the compatibility and viscosity of the product, and improves the transmission quality of optical fibers.
Preferably, the base oil is one or more of a secondary hydrogenated paraffinic base oil, a tertiary hydrogenated paraffinic base oil, and a synthetic oil.
By adopting the technical scheme and using proper base oil, the prepared hydrogen absorption optical fiber filling paste has better compatibility and more excellent thixotropic property, better protects an optical cable in the using process, improves the optical fiber transmission quality and improves the product market competitiveness.
Preferably, the organic thickener is one or more of styrene-butadiene, styrene-butadiene/propylene, styrene-butadiene/ethylene, styrene-butadiene-styrene, styrene-ethylene/butylene-styrene, styrene-ethylene/propylene-styrene, and ethylene propylene diene monomer.
By adopting the technical scheme, the organic thickening agent is selected, so that the viscosity of the product can be improved, the buffering effect of the product is improved, the optical cable is better protected in the using process, the optical fiber transmission quality is improved, and the market competitiveness of the product is improved.
Preferably, the antioxidant is a multi-hindered phenol antioxidant, the dispersion stabilizer is propylene glycol or polyethylene glycol, and the pour point depressant is a polymethacrylate pour point depressant.
By adopting the technical scheme and selecting a proper dispersing agent, raw materials in the product are dispersed more uniformly, and the viscosity and thixotropy of the product are improved; the antioxidant performance of the product can be improved by using a proper antioxidant, the low-temperature resistance of the product can be improved by using a proper pour point depressant, the product can keep stable performance under a low-temperature condition, the application range of the product is improved, and the market competitiveness of the product is improved.
In order to achieve the second object, the invention provides the following technical scheme: a production process of OPGW hydrogen absorption optical fiber filling paste comprises the following steps:
(1) removing steam: weighing the base oil according to a set proportion, heating to 120-130 ℃, and carrying out steam removal treatment for 60-120 min to obtain pure oil;
(2) mixing and dissolving: adding an organic thickener into the pure oil, stirring, adjusting the rotating speed to be 500-1000 r/min, and mixing and dissolving at 110-130 ℃ for 60-120 min to prepare viscous oil;
(3) dispersing: cooling the viscous oil to not higher than 80 ℃, adding an antioxidant, a dispersion stabilizer and a pour point depressant, and continuously stirring at the rotating speed of 500-800 rpm for 60-120 min to prepare stable oil;
(4) hydrogen absorption treatment: cooling the stabilized oil to 40-50 deg.C, adding hydrogen absorbing material, and stirring at 500-800 rpm for 60-120 min to obtain hydrogen absorbing ointment;
(5) air extraction: stopping stirring, and vacuumizing the hydrogen absorption ointment for 60-120 min to obtain the OPGW hydrogen absorption optical fiber filling ointment product.
By adopting the technical scheme, moisture in the base oil can be removed through steam removal, bubbles in the product can be removed through air extraction, moisture can be prevented from corroding the optical fiber, the service life of the optical cable is prolonged, and the market competitiveness of the product is improved; the base oil and the organic thickening agent are mixed and dissolved through the mixing and dissolving step, so that the thickening agent is more uniformly dispersed in a product, the viscosity and the thixotropy of the product are better improved, the optical fiber is always in the most free stress-free state, the microbending loss of the optical fiber and the stress corrosion of the optical fiber under the action of stress, moisture and humidity are reduced, the transmission quality of the optical fiber is improved, the service life of the optical cable is prolonged, and the market competitiveness of the product is improved.
Preferably, the step (4) comprises the following steps:
(4A) dipping: weighing silver nitrate according to a set proportion, wherein the weight ratio of silver nitrate: adding water in a ratio of 1:1-30, stirring to dissolve silver nitrate, adding a molecular sieve, uniformly stirring, and standing for 30-90 min to obtain a wet molecular sieve material;
(4B) roasting: drying the wet molecular sieve material at 60-100 ℃ for 30-100 min, heating to 500-600 ℃ and roasting for 1-4 h to prepare a hydrogen absorption material;
(4C) preparing the ointment: and (4) cooling the stable oil prepared in the step (3) to 40-50 ℃, adding the hydrogen absorption material prepared in the step (4B), and continuously stirring at the rotating speed of 500-800 rpm for 60-120 min to prepare the hydrogen absorption ointment.
By adopting the technical scheme, silver ions are uniformly adsorbed on the molecular sieve through impregnation, silver nitrate is subjected to decomposition reaction to generate silver oxide through roasting, the mobility of the silver ions is reduced, the silver ions are locked on the molecular sieve, the silver ions serving as active components are not easy to run off from the molecular sieve, and the silver ions and the molecular sieve can better play a synergistic effect, so that the hydrogen absorption function of the hydrogen absorption material is better played, the hydrogen absorption performance of a product is improved, and the market competitiveness of the product is improved.
Preferably, the step (4A) adopts an equal-volume impregnation method, critical water absorption rate of the molecular sieve before the molecular sieve can flow after being added with water is calculated through experiments, the molecular sieve with required weight is weighed, water absorption capacity of the molecular sieve is calculated through the critical water absorption rate, water with the same quantity as the water absorption capacity is weighed, silver nitrate is dissolved in the water, the molecular sieve is added, the mixture is uniformly stirred, and the molecular sieve wet material is prepared through static impregnation for 30-90 min.
By adopting the technical scheme, silver ions are adsorbed on the molecular sieve by adopting an equal-volume impregnation method, the condition of insufficient water amount or excessive water amount is avoided, if the used water is excessive, excessive water which is not adsorbed on the molecular sieve contains a certain amount of silver ions, so that the silver ions are unevenly dispersed on the molecular sieve, if the used water is insufficient, a part of the molecular sieve cannot adsorb water, namely a part of the molecular sieve cannot adsorb the silver ions, and the silver ions are not favorably and uniformly distributed on the hydrogen absorption material. The method adopts an isometric impregnation method, is beneficial to the uniform distribution of silver ions on the molecular sieve, and better plays the synergistic action of the silver ions and the molecular sieve, thereby better playing the hydrogen absorption function of the hydrogen absorption material, improving the hydrogen absorption performance of the product and improving the market competitiveness of the product.
In summary, the invention includes at least one of the following beneficial technical effects:
1. according to the invention, the silver molecular sieve hydrogen absorption material is used, in the using process, hydrogen is firstly absorbed on the molecular sieve material with high specific surface area, and hydrogen atoms in the hydrogen react with oxygen elements in any form under the catalytic action of silver ions to generate water which is stored in the molecular sieve pore channel, so that the hydrogen concentration around the optical fiber is obviously reduced, the adverse effect of the hydrogen on the optical fiber transmission quality is obviously reduced, and the optical fiber transmission quality is improved; the silica aluminate molecular sieve has strong adhesive property and better compatibility with base oil, can be better bonded with filling paste raw materials such as the base oil, improves the compatibility, the viscosity and the thixotropy of products, better protects optical fibers and improves the transmission quality of the optical fibers;
2. the HY molecular sieve with high specific surface area is used, has larger pore volume and better adsorption performance on hydrogen, and is cooperated with silver ions to convert the hydrogen more quickly, so that the hydrogen absorption effect is better exerted, and the hydrogen absorption performance of the product is improved; the HY molecular sieve with small particle size has larger external surface area, larger contact area with other raw materials in the filling paste, stronger adhesion capability, improved product compatibility, viscosity and thixotropy, better optical fiber protection, improved optical fiber transmission quality and improved product market competitiveness;
3. according to the invention, silver nitrate is adsorbed on the molecular sieve through an impregnation method, and then the silver nitrate is decomposed to generate silver oxide through high-temperature roasting, so that the fluidity of silver ions is reduced, the silver ions are better locked on the molecular sieve, the synergistic effect of the silver ions and the molecular sieve is better played, the hydrogen absorption performance of the product is improved, and the market competitiveness of the product is improved.
Detailed Description
Examples
The present invention will be described in further detail below.
Example 1: a production process of OPGW hydrogen absorption optical fiber filling paste comprises the following steps:
(1) removing steam: weighing 85g of tertiary hydrogenated paraffin base oil, transferring the tertiary hydrogenated paraffin base oil into a reaction bottle, heating to 125 ℃, and carrying out steam removal treatment for 1.5 hours to obtain pure oil;
(2) mixing and dissolving: adding 12g of styrene-ethylene/butylene-styrene polymer organic thickening agent into the pure oil, stirring, adjusting the rotating speed to 750 revolutions per minute, and mixing and dissolving at 120 ℃ for 1.5 hours to prepare viscous oil;
(3) dispersing: cooling the viscous oil to 75 ℃, adding 0.5g of multi-component hindered phenol antioxidant, 0.5g of propylene glycol dispersion stabilizer and 1.0g of polymethacrylate pour point depressant, and continuously stirring at the rotating speed of 650 revolutions per minute for 1.5 hours to prepare stable oil;
(4) hydrogen absorption treatment, comprising the following steps: (4A) dipping: grinding HY molecular sieve with specific surface area of 705 square meter/g, sieving with vibration sieve with pore size of 0.2-2 μm and pore size of 2 μm, and selecting HY molecular sieve particle with particle size of 0.2-2 μm; adopting an isometric immersion method, calculating the required water amount through a water absorption experiment, weighing 0.55g of silver nitrate, adding into 3.5g of water, stirring until the silver nitrate is completely dissolved, adding 2.2g of HY type molecular sieve, stirring uniformly, and statically immersing for 60min to obtain a molecular sieve wet material; (4B) roasting: drying the wet molecular sieve material at 80 ℃ for 65min, heating to 550 ℃, and roasting for 2.5h to obtain a hydrogen absorption material; (4C) preparing the ointment: cooling the stabilized oil prepared in the step (3) to 45 ℃, adding the hydrogen absorption material prepared in the step (4B), and continuously stirring at the rotating speed of 650 revolutions per minute for 1.5 hours to prepare hydrogen absorption ointment;
(5) air extraction: stopping stirring, vacuumizing the reaction bottle until the pressure in the reaction bottle is-0.09 MPa, and carrying out vacuum treatment on the hydrogen-absorbing ointment for 1.5h to obtain the OPGW hydrogen-absorbing optical fiber filling ointment product.
Example 2
Example 2 differs from example 1 in that example 2 uses a ZSM-5 molecular sieve instead of an HY type molecular sieve, the ZSM-5 molecular sieve having a specific surface area of 405 square meters per gram, all other things remaining in agreement with example 1.
Example 3
Example 3 differs from example 1 in that example 3 used an equal mass of the second hydrogenated paraffinic base oil instead of the third hydrogenated paraffinic base oil, and the rest was the same as example 1.
Example 4
Example 4 differs from example 1 in that example 4 uses an equal mass of polyalphaolefin synthetic oil instead of the tertiary hydrogenated paraffinic base oil, all otherwise consistent with example 1.
Example 5
Example 5 is different from example 1 in that example 5 uses an equal mass of a styrene-butadiene-based organic thickener instead of a styrene-ethylene/butylene-styrene polymer-based organic thickener, and the others are in accordance with example 1.
Example 6
Example 6 differs from example 1 in that example 6 uses an equal mass of styrene-butadiene/propylene-based organic thickener instead of a styrene-ethylene/butylene-styrene polymer-based organic thickener, all otherwise consistent with example 1.
Example 7
Example 7 is different from example 1 in that example 7 uses an equal mass of a polyethylene glycol-based dispersion stabilizer instead of a propylene glycol-based dispersion stabilizer, and the others are in accordance with example 1.
Example 8
Example 8 differs from example 1 in that example 8 was carried out without using the impregnation method to prepare a hydrogen absorbing material, 0.55g of silver oxide powder and 2.2g of an HY type molecular sieve were directly mixed uniformly, ball milling was carried out to prepare a hydrogen absorbing material, the hydrogen absorbing material was added to the stabilizing oil obtained in step (3) of example 8, the temperature was reduced to 45 ℃, stirring was continued at 650 rpm for 1.5 hours to prepare a hydrogen absorbing ointment, and the rest was identical to example 1.
Example 9
Example 9 differs from example 1 in that example 9 does not use an equal volume impregnation method, and the amount of water used for impregnation is 20% more than the theoretical water absorption of an HY type molecular sieve, all other things being consistent with example 1.
Example 10
Example 10 differs from example 1 in that example 10 does not use an equivalent volume impregnation method, and the amount of water used for impregnation is 20% less than the theoretical water absorption of an HY type molecular sieve, all other things being consistent with example 1.
Examples 11 to 18
Examples 11-18 differ from example 1 in the amounts of starting materials added and the process parameters of examples 11-18. The amounts of the starting materials used in examples 11 to 18 are shown in Table 1, and the process parameters for examples 11 to 18 are shown in Table 2.
TABLE 1 addition of the starting materials of examples 11 to 18
Figure BDA0002456227920000071
TABLE 2 parameters in the procedure of examples 11-18
Figure BDA0002456227920000072
Figure BDA0002456227920000081
Comparative example
Comparative example 1
The difference between the comparative example 1 and the example 1 is that no silver molecular sieve hydrogen absorption material is added in the comparative example 1, after the step (3) of the comparative example 1 is completed, the temperature is reduced to 45 ℃, the stirring is stopped, the reaction bottle is vacuumized until the pressure in the reaction bottle is-0.09 MPa, and the hydrogen absorption ointment is vacuumized for 1.5 hours to prepare the product, wherein the rest is consistent with the example 1.
Comparative example 2
The difference between the comparative example 2 and the example 1 is that the comparative example 2 does not add silver nitrate, after the step (3) of the comparative example 2 is completed, the temperature is reduced to 45 ℃, 2.2g of HY molecular sieve is added, and the stirring is continued for 1.5h at the rotation speed of 650 revolutions per minute, so as to prepare the hydrogen absorbing ointment, and the rest is consistent with the example 1.
Comparative example 3
Comparative example 3 is different from example 1 in that in comparative example 3, silver oxide was directly used as a hydrogen absorbing material without adding a molecular sieve, and after step (3) of comparative example 3 was completed, the temperature was decreased to 45 ℃, 0.44g of silver oxide was added, and stirring was continued at 650 rpm for 1.5 hours to prepare a hydrogen absorbing ointment, and the others were all in accordance with example 1.
Comparative example 4
Comparative example 4 differs from example 1 in that comparative example 4 uses an equal mass of activated carbon instead of an HY type molecular sieve, all otherwise in keeping with example 1.
Comparative example 5
Comparative example 5 differs from example 1 in that comparative example 5 used equal mass of activated carbon instead of HY type molecular sieve and 0.03g of palladium nitrate instead of 0.55g of silver nitrate, all in keeping with example 1.
Performance detection
The OPGW hydrogen absorption optical fiber filling paste products prepared in the examples 1-18 and the comparative examples 1-5 are sent to be tested for hydrogen absorption performance and compatibility performance. Hydrogen absorption performance test reference is made to YD/T839.1-2015 "filling and coating compound for telecommunication cables cable first part: test method the test method of hydrogen absorption performance of the hydrogen absorption type filling compound disclosed in appendix I of the test methods is tested for 24 hours at 23 ℃ and standard atmospheric pressure, the hydrogen absorption amount is calculated, and the test results are shown in Table 3. The compatibility testing method is as follows: putting 5g of a hydrogen absorption optical fiber filling paste sample into a centrifugal tube of a high-speed centrifuge, centrifuging for 10min at the rotating speed of 4000 revolutions per minute, observing whether the delamination phenomenon or the solid precipitation occurs or not after centrifuging, if the delamination phenomenon does not occur and the solid precipitation does not occur, centrifuging for 10min again after the rotating speed is increased to 4500 revolutions per minute to perform a speed-up experiment, if the delamination phenomenon does not occur and the solid precipitation does not occur, repeating the speed-up experiment process at the speed-up increased speed of 500 revolutions per minute each time until the delamination phenomenon or the solid precipitation occurs, recording the rotating speed when the delamination phenomenon or the solid precipitation occurs, namely the critical rotating speed of the product, wherein the higher the critical rotating speed is, the better the product compatibility is, the better the product stability is, and the test results.
TABLE 3 comparison table of performance test results of different OPGW hydrogen absorption optical fiber filling paste products
Figure BDA0002456227920000091
Figure BDA0002456227920000101
Comparative example 1 under the experimental condition that the hydrogen absorption material of the silver molecular sieve is not added, the prepared product has high centrifugal critical rotation speed and good product stability and compatibility, but the hydrogen absorption performance is poor, the transmission quality of the optical fiber can be influenced, the market popularization of the product is not facilitated, and the market competitiveness of the product is poor. In the comparative example 2, the prepared product has good stability and compatibility under the conditions of not adding silver nitrate and only adding the molecular sieve, but has poor hydrogen absorption performance, can influence the transmission quality of the optical fiber, is not beneficial to the market popularization of the product, and has poor market competitiveness of the product. Comparative example 3 no molecular sieve is added, silver oxide is directly used as hydrogen absorption material, and the prepared product has good stability and compatibility, but the hydrogen absorption performance is poor, the transmission quality of the optical fiber is affected, the market popularization of the product is not facilitated, and the market competitiveness of the product is poor. Comparative example 4 the same quality of activated carbon is used to replace HY molecular sieve, and the prepared product has certain hydrogen absorption performance, but the critical temperature of centrifugal treatment is low, the stability and compatibility of the product are poor, and the market popularization of the product is not facilitated. Compared with the prior art, the method has the advantages that the prepared product has stronger hydrogen absorption performance by using the equal-mass activated carbon instead of the HY molecular sieve and using 0.03g of palladium nitrate instead of 0.55g of silver nitrate, but the critical temperature of centrifugal treatment is low, the stability and compatibility of the product are poor, and the market popularization of the product is not facilitated.
Comparing the experimental results of the embodiment 1 and the comparative examples 1 to 5, it can be seen that, in the process of preparing the OPGW hydrogen absorption optical fiber filling paste, a hydrogen absorption material prepared by using an HY type molecular sieve and silver nitrate by using an equal volume impregnation method is added, the OPGW hydrogen absorption optical fiber filling paste prepared in the embodiment 1 has excellent hydrogen absorption performance, the critical rotation speed of product centrifugal treatment is high, the product stability and compatibility are good, the optical fiber can be better protected, the service life is prolonged, the transmission quality of the optical fiber is improved to a certain extent, and the product market competitiveness is good.
Comparing the experimental results of example 1 and example 2, in example 2, ZSM-5 molecular sieve is used instead of HY-type molecular sieve, the hydrogen absorption performance of the prepared OPGW hydrogen absorption optical fiber filling paste product is reduced, the critical rotation speed of the product centrifugal treatment is reduced, the product stability and compatibility are reduced, the protection effect on the optical fiber is reduced, and the service life of the product is affected. Therefore, the preferred embodiment of the present invention is to use an HY type molecular sieve with small particle size and large specific surface area.
Comparing the experimental results of the embodiment 1 and the embodiments 3-4, the embodiments 3-4 select different types of base oil, and the prepared OPGW hydrogen absorption optical fiber filling paste product has excellent hydrogen absorption performance, good product stability and compatibility, and excellent market competitiveness.
Comparing the experimental results of example 1 and examples 5-6, examples 5-6 use different types of organic thickeners, and the prepared OPGW hydrogen absorption optical fiber filling paste product has excellent hydrogen absorption performance, good product stability and compatibility, and excellent market competitiveness.
Comparing the experimental results of example 1 and example 7, in example 7, different types of dispersion stabilizers are selected, and the prepared OPGW hydrogen absorption optical fiber filling paste product has excellent hydrogen absorption performance, good product stability and compatibility, and excellent market competitiveness.
Comparing the experimental results of example 1 and example 8, in example 8, the hydrogen absorbing material is prepared by mechanically mixing silver oxide powder and HY-type molecular sieve without using an immersion method, the hydrogen absorbing performance of the prepared OPGW hydrogen absorbing optical fiber filling paste product is weakened, the critical rotation speed of the product centrifugal treatment is reduced, the product compatibility and stability are reduced, and the market popularization of the product is not facilitated. Comparing the experimental results of example 1 and examples 9-10, in examples 9 and 10, the hydrogen absorbing material was prepared without using an equal volume impregnation method, and the water usage was 1.2 times and 0.8 times of the theoretical water absorption capacity of the HY-type molecular sieve, respectively, and the hydrogen absorption performance of the prepared OPGW hydrogen absorbing optical fiber filling paste product was slightly reduced, which was not favorable for the market promotion of the product. Therefore, a preferred embodiment of the present invention is to use an isovolumetric impregnation method for preparing the hydrogen absorbing material.
Examples 11-18 have different amounts of starting materials and different process parameters compared to example 1. Wherein the weight ratio of the raw materials of the embodiments 15-18 is as follows: 80-90 parts of base oil, 5-15 parts of organic thickening agent, 0.3-0.8 part of antioxidant, 0.2-0.8 part of dispersion stabilizer, 0.5-1.5 parts of pour point depressant, 0.4-4 parts of HY type molecular sieve and 0.1-1 part of silver nitrate; the OPGW hydrogen absorption optical fiber filling paste products prepared in the embodiments 15-18 have excellent hydrogen absorption performance, higher centrifugal treatment critical rotation speed, better product compatibility and stability and strong market competitiveness. The weight ratio of the raw materials of examples 11-14 is different from that of examples 15-18, and the prepared OPGW hydrogen absorption optical fiber filling paste product has slightly reduced hydrogen absorption performance and slightly reduced compatibility and stability. Therefore, the preferable weight ratio of the raw materials is as follows: 80-90 parts of base oil, 5-15 parts of organic thickening agent, 0.3-0.8 part of antioxidant, 0.2-0.8 part of dispersion stabilizer, 0.5-1.5 parts of pour point depressant, 0.4-4 parts of HY type molecular sieve and 0.1-1 part of silver nitrate.
The HY molecular sieve with the particle size of more than 2 mu m can be crushed into the particle size of not more than 2 mu m and then used. The invention develops an optical fiber filling factice suitable for filling a stainless steel tube optical fiber loose tube in an OPGW optical cable, and the optical fiber filling factice can absorb hydrogen generated during welding of the stainless steel loose tube by adding a hydrogen absorbing material so as to protect an optical fiber from being lost. The product prepared by the invention has excellent hydrogen absorption performance, and the compatibility of the hydrogen absorption material and other materials in the ointment is better. Besides detecting the hydrogen absorption performance and the compatibility of the product prepared by the invention, the physical and chemical properties of the product prepared by the invention also need to meet various quality indexes specified in table 4.
TABLE 4 physicochemical Property requirements of the products of the invention
Figure BDA0002456227920000111
Figure BDA0002456227920000121
The embodiments of the present invention are preferred embodiments of the present invention, and the scope of the present invention is not limited by these embodiments, so: all equivalent changes made according to the structure, shape and principle of the invention are covered by the protection scope of the invention.

Claims (10)

1. The OPGW hydrogen absorption optical fiber filling paste is characterized by being mainly prepared from the following filling paste raw materials in parts by weight: 80-90 parts of base oil, 3-15 parts of organic thickening agent, 0.1-1 part of antioxidant, 0.1-1 part of dispersion stabilizer, 0.1-2 parts of pour point depressant and 0.1-5 parts of hydrogen absorption material, wherein the hydrogen absorption material is a silver molecular sieve.
2. The OPGW hydrogen-absorbing optical fiber filling paste as claimed in claim 1, which is mainly prepared from the following raw materials in parts by weight: 80-90 parts of base oil, 5-15 parts of organic thickening agent, 0.3-0.8 part of antioxidant, 0.2-0.8 part of dispersion stabilizer, 0.5-1.5 parts of pour point depressant and 0.5-5 parts of silver molecular sieve.
3. The OPGW hydrogen-absorbing optical fiber filling paste as claimed in claim 2, wherein the silver molecular sieve is mainly prepared from the following hydrogen-absorbing raw materials in parts by weight: 0.4-4 parts of molecular sieve and 0.1-1 part of silver nitrate.
4. The OPGW hydrogen-absorbing optical fiber filling paste as claimed in claim 3, wherein the molecular sieve is an HY type molecular sieve, the specific surface area of the HY type molecular sieve is 600 square meters per gram to 800 square meters per gram, and the particle size of the HY type molecular sieve is 0.2 μm to 2 μm.
5. The OPGW hydrogen-absorbing optical fiber filling paste as claimed in claim 1, wherein the base oil is one or more of a secondary hydrogenated paraffinic base oil, a tertiary hydrogenated paraffinic base oil and a synthetic oil.
6. The OPGW hydrogen-absorbing optical fiber filling paste as recited in claim 1, wherein: the organic thickener is one or more of styrene-butadiene, styrene-butadiene/propylene, styrene-butadiene/ethylene, styrene-butadiene-styrene, styrene-ethylene/butylene-styrene, styrene-ethylene/propylene-styrene and ethylene propylene diene monomer.
7. The OPGW hydrogen-absorbing optical fiber filling paste as recited in claim 1, wherein: the antioxidant is a multi-element hindered phenol antioxidant, the dispersion stabilizer is propylene glycol or polyethylene glycol dispersion stabilizer, and the pour point depressant is polymethacrylate pour point depressant.
8. A process for producing OPGW hydrogen-absorbing optical fiber filling paste as claimed in any one of claims 1-7, characterized by comprising the following steps:
(1) removing steam: weighing the base oil according to a set proportion, heating to 120-130 ℃, and carrying out steam removal treatment for 60-120 min to obtain pure oil;
(2) mixing and dissolving: adding an organic thickener into the pure oil, stirring, adjusting the rotating speed to be 500-1000 r/min, and mixing and dissolving at 110-130 ℃ for 60-120 min to prepare viscous oil;
(3) dispersing: cooling the viscous oil to not higher than 80 ℃, adding an antioxidant, a dispersion stabilizer and a pour point depressant, and continuously stirring at the rotating speed of 500-800 rpm for 60-120 min to prepare stable oil;
(4) hydrogen absorption treatment: cooling the stabilized oil to 40-50 deg.C, adding hydrogen absorbing material, and stirring at 500-800 rpm for 60-120 min to obtain hydrogen absorbing ointment;
(5) air extraction: stopping stirring, and vacuumizing the hydrogen absorption ointment for 60-120 min to obtain the OPGW hydrogen absorption optical fiber filling ointment product.
9. The process for producing an OPGW hydrogen-absorbing optical fiber filling paste as claimed in claim 8, wherein the step (4) comprises the steps of:
(4A) dipping: weighing silver nitrate according to a set proportion, wherein the weight ratio of silver nitrate: adding water according to the ratio of water =1:1-30, stirring to dissolve silver nitrate, adding the molecular sieve, uniformly stirring, and standing for 30-90 min to prepare a wet molecular sieve material;
(4B) roasting: drying the wet molecular sieve material at 60-100 ℃ for 30-100 min, heating to 500-600 ℃ and roasting for 1-4 h to prepare a hydrogen absorption material;
(4C) preparing the ointment: and (4) cooling the stable oil prepared in the step (3) to 40-50 ℃, adding the hydrogen absorption material prepared in the step (4B), and continuously stirring at the rotating speed of 500-800 rpm for 60-120 min to prepare the hydrogen absorption ointment.
10. The process for producing OPGW hydrogen-absorbing optical fiber filling paste as claimed in claim 9, wherein the process comprises the following steps: and (4A) adopting an isometric immersion method, calculating the critical water absorption rate of the molecular sieve before the molecular sieve can flow after being added with water through experiments, weighing the molecular sieve with the required weight, calculating the water absorption capacity of the molecular sieve through the critical water absorption rate, weighing water with the same amount as the water absorption capacity, dissolving silver nitrate in the water, adding the molecular sieve, uniformly stirring, and statically immersing for 30-90 min to prepare the molecular sieve wet material.
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Application publication date: 20200828