CN111808431A - Optical fiber filling paste with ultralow loss to optical fiber and preparation method thereof - Google Patents
Optical fiber filling paste with ultralow loss to optical fiber and preparation method thereof Download PDFInfo
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- CN111808431A CN111808431A CN202010627233.XA CN202010627233A CN111808431A CN 111808431 A CN111808431 A CN 111808431A CN 202010627233 A CN202010627233 A CN 202010627233A CN 111808431 A CN111808431 A CN 111808431A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L91/00—Compositions of oils, fats or waxes; Compositions of derivatives thereof
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/44—Mechanical structures for providing tensile strength and external protection for fibres, e.g. optical transmission cables
- G02B6/4401—Optical cables
- G02B6/4429—Means specially adapted for strengthening or protecting the cables
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/44—Mechanical structures for providing tensile strength and external protection for fibres, e.g. optical transmission cables
- G02B6/4401—Optical cables
- G02B6/4429—Means specially adapted for strengthening or protecting the cables
- G02B6/44384—Means specially adapted for strengthening or protecting the cables the means comprising water blocking or hydrophobic materials
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention discloses an optical fiber filling paste with ultralow loss for an optical fiber, which comprises the following components in percentage by weight: 75-95% of GTL base oil; 3-10% of polymer synthetic rubber; 1-6% of viscosity index improver; 1-6% of carbon nano tube; 0.3-1% of structure stabilizer; 0.3 to 1 percent of antioxidant; the sum of the weight percentage contents of the components is 100 percent; the carbon nanotube is a multi-walled carbon nanotube. The optical fiber filling paste with ultralow loss to the optical fiber and the preparation method thereof have excellent high and low temperature performance and yield stress, the optical fiber filling paste has good oxidation stability and stable structural shear, has certain strength and toughness and has excellent compatibility with optical fiber sleeve materials and tight sleeve materials, and the optical fiber filling paste can enable the optical fiber to be in the most free stress-free state in a sleeve and a cable core in a cable all the time.
Description
Technical Field
The invention relates to an optical fiber filling paste with ultralow loss for an optical fiber and a preparation method thereof.
Background
With the rapid development of information technology, the application fields such as 5G broadband networks, land trunks, marine communications and the like need to be oriented, the application and popularization of ultra-low loss optical fibers are accelerated, the serial development and design of products are promoted, the performance and the reliability are improved, and the automation, the intellectualization and the networking upgrading of production lines are promoted. At present, related industries hope to take ultra-low loss series optical fiber products as a core, drive related industries of upstream, middle and downstream to mutually fuse and collaborate, divide work and cooperate, share benefits, and promote the cooperative development of an industrial chain.
The industry puts forward new requirements on the key material optical fiber filling paste for preparing the ultra-low loss optical cable: the specific targets are as follows:
1. the high-performance optical fiber loose tube filling factice and related optical cable structure materials realize good compatibility;
2. the oxidation induction period of the optical fiber ointment is more than or equal to 30 minutes;
3. the yield stress of the optical fiber ointment reaches 66.2 Pa;
4. at the low temperature of minus 40 ℃, the cone penetration of the optical fiber ointment is more than or equal to 2301/10 mm;
5. the optical fiber ointment keeps the stability of the colloid structure and does not generate dripping when the temperature is 80 ℃.
Disclosure of Invention
The invention aims to solve the problems and provides an optical fiber filling paste with ultralow loss for an optical fiber and a preparation method thereof, wherein the optical fiber filling paste has excellent high and low temperature performance and yield stress, good stability, stable structure shearing, certain strength and toughness and excellent compatibility with an optical fiber sleeve material and a tight sleeve material, and can enable the optical fiber to be in the most free stress-free state in the sleeve and a cable core in a cable all the time.
The purpose of the invention is realized as follows:
the invention relates to an optical fiber filling paste with ultralow loss for an optical fiber, which comprises the following components in percentage by weight:
the sum of the weight percentage contents of the components is 100 percent;
the carbon nanotube is a multi-walled carbon nanotube.
In the above paste for filling an optical fiber with ultra-low loss, the polymer synthetic rubber is SEP thermoplastic rubber.
The optical fiber filling paste with ultralow loss to the optical fiber is characterized in that the viscosity index improver is SV 260.
The optical fiber filling paste with ultralow loss to the optical fiber is characterized in that the structure stabilizer is polyethylene glycol.
The optical fiber filling paste with ultralow loss to the optical fiber is characterized in that the antioxidant is a composite high-temperature liquid antioxidant.
The invention relates to a preparation method of optical fiber filling paste with ultralow loss to optical fibers, which comprises the following steps:
the method comprises the following steps: preparing raw materials according to the following components in percentage by weight:
the sum of the weight percentage contents of the components is 100 percent;
the carbon nano tube is a multi-wall carbon nano tube;
step two: adding the GTL base oil, the polymer synthetic rubber and the viscosity index improver prepared in the step one into a reaction kettle, heating while stirring, adding the antioxidant prepared in the step one into the reaction kettle when the temperature is raised to 160 ℃, stirring at constant temperature for 3-5 hours until the polymer synthetic rubber and the viscosity index improver are completely dissolved in the GTL base oil to form a master batch, transferring the master batch out of the reaction kettle, and cooling the master batch to be lower than 60 ℃ for later use;
step three: adding the cooled master batch in the step two into a stirring kettle, slowly adding the carbon nano tubes prepared in the step one into the stirring kettle, continuously stirring for 1-2 hours after the carbon nano tubes are completely soaked in the master batch, then adding the structure stabilizer prepared in the step one, and continuously stirring for 1-2 hours to form a base material;
step four: carrying out high-pressure homogenizing grinding on the base material in the third step by a high-pressure homogenizing pump, wherein the homogenizing pressure is controlled to be about 25-35 MPa;
step five: and (4) carrying out homogenizing dispersion, vacuum degassing, vacuum centrifugation, filtration and filling on the base material which is homogenized and ground under high pressure in the fourth step.
The preparation method of the optical fiber filling paste with ultralow loss of the optical fiber is characterized in that when the vacuum centrifugation is carried out in the fifth step, the centrifugal rotating speed is 2000-3500 rpm, and the vacuum negative pressure is-0.07 to-0.1 MPa.
The invention has the following advantages:
1. GTL base oil is selected to replace the traditional base oil, so that the compatibility of the optical fiber filling paste to optical cable materials is greatly improved, the compatibility of the optical cable material (PBT) and the optical fiber materials is excellent, the oil absorption rate of the optical fiber filling paste to the PBT and the optical fiber materials can be greatly reduced, the weight change rate (oil absorption rate) of common factice to the sleeve material is about 1.5 percent generally when the common factice is aged for 45x24h in an environment of 85 ℃, and the weight change rate of the optical fiber filling paste is about 0.7 percent under the aging condition. The rate of weight change (oil absorption) of conventional ointments to fiber materials is typically around 0.8% for 30x24h aged in an 85 ° environment, while the rate of weight change of the fiber filler paste is around 0.3% under the aged condition. The main reason is that GTL base oil is natural gas oil, the base oil of the common fiber paste is paraffin with a linear structure and a branched chain, and a naphthenic structure and an aromatic structure are connected to a molecular chain according to different refining degrees; GTL base oils are predominantly highly saturated straight chain alkanes with several methyl side chains, with higher levels of polar components, contributing to good compatibility. Meanwhile, the GTL base oil has a large molecular weight, has a large molecular structure difference with a cable loose tube material (PBT), and avoids the solvation tendency; naphthenic base oils generally used in the art have a molecular ratio of naphthenic structure as high as 40 to 70%, hydrorefined base oils (hydrogenated white oils) are composed of paraffins and naphthenes having long and short non-uniform branches, and PAO synthetic oils have highly long-branched paraffinic structures and are prone to solvation.
2. The multi-walled carbon nanotube is applied to the factice industry for the first time, the material belongs to a high-strength and high-toughness carbon fiber material, and the yield stress of the optical fiber factice can be greatly improved when the material is applied to the factice. The stress mainly plays a role in protecting the optical fiber in time once the optical fiber is subjected to external force, and the optical fiber cannot generate any signal transmission in a free state; meanwhile, the conventional mode of adding the multi-walled carbon nanotubes can only play a relatively common toughening and reinforcing effect, and the multi-walled carbon nanotubes are better dispersed in the optical fiber filling paste by the vacuum centrifugal operation in the fifth step, so that the optical fiber filling paste forms a three-dimensional network structure finally, and the toughening and reinforcing effect is further enhanced.
Drawings
FIG. 1 is a flow chart illustrating the preparation of the ultra-low loss optical fiber filling paste according to the present invention.
Detailed Description
The invention relates to an optical fiber filling paste with ultralow loss for an optical fiber, which comprises the following components in percentage by weight:
the sum of the weight percentage contents of the components is 100 percent;
the carbon nano tube is a multi-wall carbon nano tube;
preferably, the polymer synthetic rubber is SEP thermoplastic rubber;
preferably, the viscosity index improver is SV 260;
preferably, the structure stabilizer is polyethylene glycol;
the invention relates to a preparation method of optical fiber filling paste with ultralow loss to optical fibers, which comprises the following steps:
the method comprises the following steps: preparing raw materials according to the following components in percentage by weight:
the sum of the weight percentage contents of the components is 100 percent;
the carbon nano tube is a multi-wall carbon nano tube;
step two: adding the GTL base oil, the polymer synthetic rubber and the viscosity index improver prepared in the step one into a reaction kettle, heating while stirring, adding the antioxidant prepared in the step one into the reaction kettle when the temperature is raised to 160 ℃, stirring at constant temperature for 3-5 hours until the polymer synthetic rubber and the viscosity index improver are completely dissolved in the GTL base oil to form a master batch, transferring the master batch out of the reaction kettle, and cooling the master batch to be lower than 60 ℃ for later use;
step three: adding the cooled master batch in the step two into a stirring kettle, slowly adding the carbon nano tubes prepared in the step one into the stirring kettle, continuously stirring for 1-2 hours after the carbon nano tubes are completely soaked in the master batch, then adding the structure stabilizer prepared in the step one, and continuously stirring for 1-2 hours to form a base material;
step four: carrying out high-pressure homogenizing grinding on the base material in the third step by a high-pressure homogenizing pump, wherein the homogenizing pressure is controlled to be 25-35 MPa;
step five: and (4) carrying out homogenizing dispersion, vacuum degassing, vacuum centrifugation, filtration and filling on the base material which is homogenized and ground under high pressure in the fourth step.
Preferably, when the vacuum centrifugation is performed in the step five, the centrifugation rotating speed is 2000-.
The present invention will be further described with reference to FIG. 1, examples 1-4 and comparative examples 1-3, wherein the preparation of examples 1-4 is shown in FIG. 1.
The information on the raw materials used in examples 1 to 4 of the present invention and comparative examples 1 to 3 is as follows:
GTL base oil: shell (China) Inc., Risella X420;
polymer synthetic rubber: zhejiang Zhongli synthetic materials science and technology, Inc., brand: m7401;
viscosity index improver: runing alliako chemistry (shenzhen) ltd, brand: SV 260;
carbon nanotube: chengdu Zhongke age nano energy science and technology Limited, brand: a multi-walled carbon nanotube;
structure stabilizer: shanghai Taoism general chemical International trade, Inc., brand: PEG 400;
antioxidant: shanghai Shihua Xinie chemical technology Co., Ltd., brand: ST-1135D liquid antioxidant.
Example 1
(1) Putting 885 g of GTL base oil into a reaction kettle, putting 70 g of measured SEP thermoplastic rubber and 20 g of SV260 viscosity index improver into the reaction kettle, heating while stirring, adding 5g of measured antioxidant when the temperature is increased to 160 ℃, stirring for 3-5 hours at constant temperature until the SEP thermoplastic rubber and the SV260 viscosity index improver are completely dissolved in the GTL base oil to form a master batch, then moving the master batch out of the reaction kettle, and cooling to the temperature lower than 60 ℃ for later use;
(2) adding the cooled master batch into a stirring kettle, slowly adding 15 g of the measured multi-walled carbon nanotubes into the stirring kettle, sequentially stirring while adding, stirring for 1-2 hours after the multi-walled carbon nanotubes are completely soaked in the master batch, adding 5g of PEG400 type structure stabilizer, and continuously stirring for 1-2 hours to form a base material;
(3) and (3) carrying out high-pressure homogenizing grinding on the base material by a high-pressure homogenizing pump, wherein the homogenizing pressure is controlled at 30 MPa.
(4) And (3) carrying out homogeneous dispersion, vacuum degassing, vacuum centrifugation, filtration and filling on the base material after the homogeneous grinding to obtain the sample of the example 1. When vacuum centrifugation is carried out, the centrifugal rotating speed is 2000 r/min, the vacuum negative pressure is-0.08 MPa, and the optical fiber filling paste with the three-dimensional net structure is finally prepared by utilizing the principle that the centrifugal force is greater than the vacuum negative pressure difference.
The samples of example 1 were tested for the following main technical criteria, the results of which are shown in table 1 below:
TABLE 1 test results of the main technical index of the sample of example 1
| Serial number | Inspection item | Unit of | Standard requirements | Test results |
| 1 | Appearance of the product | / | Homogeneous, free of extraneous matter | Qualified |
| 2 | Cone penetration (-40 ℃ C.) | 1/10mm | ≥230 | 280 |
| 3 | Oil separating (80 ℃, 24h) | ％ | ≤0.5 | 0 |
| 4 | High temperature stability at 80 deg.C | 24h | —— | By passing |
| 5 | Oxidative induction period (190 ℃ C.) | min | ≥20 | 60 |
| 6 | Yield stress (25 ℃ C.) | pa | —— | 67 |
| 7 | PBT weight ratio (85 ℃, 45X24 h) | ％ | ≤3 | 0.7 |
| 8 | Optical fiber weight ratio (85 ℃, 30X24 h) | ％ | —— | 0.3 |
Example 2
(1) Putting 879 g of GTL base oil into a reaction kettle, putting 65 g of measured SEP thermoplastic rubber and 25 g of SV260 viscosity index improver into the reaction kettle, heating while stirring, adding 5g of measured antioxidant when the temperature is increased to 160 ℃, stirring for 3-5 hours at constant temperature until the SEP thermoplastic rubber and the SV260 viscosity index improver are completely dissolved in the GTL base oil to form a master batch, then moving the master batch out of the reaction kettle, and cooling to below 60 ℃ for later use;
(2) adding the cooled master batch into a stirring kettle, slowly adding 20 g of the measured multi-walled carbon nanotubes into the stirring kettle, sequentially stirring while adding, stirring for 1-2 hours after the multi-walled carbon nanotubes are completely soaked in the master batch, adding 6 g of PEG400 type structure stabilizer, and continuously stirring for 1-2 hours to form a base material;
(3) and (3) carrying out high-pressure homogenizing grinding on the base material by a high-pressure homogenizing pump, wherein the homogenizing pressure is controlled at 30 MPa.
(4) And (3) carrying out homogeneous dispersion, vacuum degassing, vacuum centrifugation, filtration and filling on the base material after the homogeneous grinding to obtain the sample of the example 2. When vacuum centrifugation is carried out, the centrifugal rotating speed is 2000 r/min, the vacuum negative pressure is-0.08 MPa, and the optical fiber filling paste with the three-dimensional net structure is finally prepared by utilizing the principle that the centrifugal force is greater than the vacuum negative pressure difference.
The samples of example 2 were tested for the following main technical criteria, the results of which are shown in table 2 below:
table 2 main technical index test results of the sample of example 2
| Serial number | Inspection item | Unit of | Standard requirements | Test results |
| 1 | Appearance of the product | / | Homogeneous, free of extraneous matter | Qualified |
| 2 | Cone penetration (-40 ℃ C.) | 1/10mm | ≥230 | 276 |
| 3 | Oil separating (80 ℃, 24h) | ％ | ≤0.5 | 0 |
| 4 | High temperature stability at 80 deg.C | 24h | —— | By passing |
| 5 | Oxidative induction period (190 ℃ C.) | min | ≥20 | 60 |
| 6 | Yield stress (25 ℃ C.) | pa | —— | 68 |
| 7 | PBT weight ratio (85 ℃, 45X24 h) | ％ | ≤3 | 0.65 |
| 8 | Optical fiber weight ratio (85 ℃, 30X24 h) | ％ | —— | 0.28 |
Example 3
(1) 872 g of GTL base oil is put into a reaction kettle, then 60 g of measured SEP thermoplastic rubber and 30 g of SV260 viscosity index improver are put into the reaction kettle, then heating and stirring are carried out, when the temperature is raised to 160 ℃, 6 g of measured antioxidant is added, stirring is carried out for 3-5 hours at constant temperature until the SEP thermoplastic rubber and the SV260 viscosity index improver are completely dissolved in the GTL base oil to form a master batch, then the master batch is moved out of the reaction kettle and cooled to be lower than 60 ℃ for standby;
(2) adding the cooled master batch into a stirring kettle, slowly adding 25 g of the measured multi-walled carbon nanotubes into the stirring kettle, sequentially stirring while adding, stirring for 1-2 hours after the multi-walled carbon nanotubes are completely soaked in the master batch, adding 7 g of PEG400 type structure stabilizer, and continuously stirring for 1-2 hours to form a base material;
(3) and (3) carrying out high-pressure homogenizing grinding on the base material by a high-pressure homogenizing pump, wherein the homogenizing pressure is controlled at 30 MPa.
(4) And (3) carrying out homogeneous dispersion, vacuum degassing, vacuum centrifugation, filtration and filling on the base material after the homogeneous grinding to obtain the sample of the example 3. When vacuum centrifugation is carried out, the centrifugal rotating speed is 2000 r/min, the vacuum negative pressure is-0.08 MPa, and the optical fiber filling paste with the three-dimensional net structure is finally prepared by utilizing the principle that the centrifugal force is greater than the vacuum negative pressure difference.
The samples of example 3 were tested for the following main technical indicators, the results of which are shown in table 3 below:
TABLE 3 test results of the main technical indicators of the samples of example 3
| Serial number | Inspection item | Unit of | Standard requirements | Test results |
| 1 | Appearance of the product | / | Homogeneous, free of extraneous matter | Qualified |
| 2 | Cone penetration (-40 ℃ C.) | 1/10mm | ≥230 | 270 |
| 3 | Oil separating (80 ℃, 24h) | ％ | ≤0.5 | 0 |
| 4 | High temperature stability at 80 deg.C | 24h | —— | By passing |
| 5 | Oxidative induction period (190 ℃ C.) | min | ≥20 | 60 |
| 6 | Yield stress (25 ℃ C.) | pa | —— | 69.5 |
| 7 | PBT weight ratio (85 ℃, 45X24 h) | ％ | ≤3 | 0.55 |
| 8 | Optical fiber weight ratio (85 ℃, 30X24 h) | ％ | —— | 0.25 |
Example 4
(1) 871 g of GTL base oil is put into a reaction kettle, 55 g of measured SEP thermoplastic rubber and 30 g of SV260 viscosity index improver are put into the reaction kettle, then heating and stirring are carried out, when the temperature is raised to 160 ℃, 6 g of measured antioxidant is added, stirring is carried out for 3-5 hours at constant temperature until the SEP thermoplastic rubber and the SV260 viscosity index improver are completely dissolved in the GTL base oil to form master batch, then the master batch is moved out of the reaction kettle and cooled to be lower than 60 ℃ for standby;
(2) adding the cooled master batch into a stirring kettle, slowly adding 30 g of the measured multi-walled carbon nanotubes into the stirring kettle, sequentially stirring while adding, stirring for 1-2 hours after the multi-walled carbon nanotubes are completely soaked in the master batch, adding 8 g of PEG400 type structure stabilizer, and continuously stirring for 1-2 hours to form a base material;
(3) and (3) carrying out high-pressure homogenizing grinding on the base material by a high-pressure homogenizing pump, wherein the homogenizing pressure is controlled at 30 MPa.
(4) And (3) carrying out homogeneous dispersion, vacuum degassing, vacuum centrifugation, filtration and filling on the base material after the homogeneous grinding to obtain the sample of the example 4. When vacuum centrifugation is carried out, the centrifugal rotating speed is 2000 r/min, the vacuum negative pressure is-0.08 MPa, and the optical fiber filling paste with the three-dimensional net structure is finally prepared by utilizing the principle that the centrifugal force is greater than the vacuum negative pressure difference.
The samples of example 4 were tested for the following main technical criteria, the results of which are shown in table 4 below:
table 4 main technical index test results of the sample of example 4
| Serial number | Inspection item | Unit of | Standard requirements | Test results |
| 1 | Appearance of the product | / | Homogeneous, free of extraneous matter | Qualified |
| 2 | Cone penetration (-40 ℃ C.) | 1/10mm | ≥230 | 265 |
| 3 | Oil separating (80 ℃, 24h) | ％ | ≤0.5 | 0 |
| 4 | High temperature stability at 80 deg.C | 24h | —— | By passing |
| 5 | Oxidative induction period (190 ℃ C.) | min | ≥20 | 60 |
| 6 | Yield stress (25 ℃ C.) | pa | —— | 72 |
| 7 | PBT weight ratio (85 ℃, 45X24 h) | ％ | ≤3 | 0.5 |
| 8 | Optical fiber weight ratio (85 ℃, 30X24 h) | ％ | —— | 0.23 |
Comparative example 1
(1) Putting 885 g of hydrogenated white oil with similar viscosity (150N) into a reaction kettle, putting 70 g of measured SEP thermoplastic rubber and 20 g of SV260 viscosity index improver into the reaction kettle, heating while stirring, adding 5g of measured antioxidant when the temperature is increased to 160 ℃, stirring at constant temperature for 3-5 hours until the SEP thermoplastic rubber and the SV260 viscosity index improver are completely dissolved in the hydrogenated white oil to form a master batch, then removing the master batch from the reaction kettle, and cooling to the temperature lower than 60 ℃ for later use;
(2) adding the cooled master batch into a stirring kettle, slowly adding 15 g of the measured multi-walled carbon nanotubes into the stirring kettle, sequentially stirring while adding, stirring for 1-2 hours after the multi-walled carbon nanotubes are completely soaked in the master batch, adding 5g of PEG400 type structure stabilizer, and continuously stirring for 1-2 hours to form a base material;
(3) and (3) carrying out high-pressure homogenizing grinding on the base material by a high-pressure homogenizing pump, wherein the homogenizing pressure is controlled at 30 MPa.
(4) And (3) carrying out homogeneous dispersion, vacuum degassing, vacuum centrifugation, filtration and filling on the base material after the homogeneous grinding to obtain the sample of the comparative example 1. When vacuum centrifugation is carried out, the centrifugal rotating speed is 2000 r/min, and the vacuum negative pressure is-0.08 MPa.
The following main technical criteria were tested on the sample of comparative example 1, and the results are shown in table 5 below:
TABLE 5 main technical index test results of the sample of comparative example 1
Comparative example 2
(1) Putting 879 g of GTL base oil into a reaction kettle, putting 65 g of measured SEP thermoplastic rubber and 25 g of SV260 viscosity index improver into the reaction kettle, heating while stirring, adding 5g of measured antioxidant when the temperature is increased to 160 ℃, stirring for 3-5 hours at constant temperature until the SEP thermoplastic rubber and the SV260 viscosity index improver are completely dissolved in the GTL base oil to form a master batch, then moving the master batch out of the reaction kettle, and cooling to below 60 ℃ for later use;
(2) adding the cooled master batch into a stirring kettle, adding 6 g of PEG400 type structure stabilizer, and continuing stirring for 1-2 hours to form a base material;
(3) and (3) carrying out high-pressure homogenizing grinding on the base material by a high-pressure homogenizing pump, wherein the homogenizing pressure is controlled at 30 MPa.
(4) And (3) carrying out homogeneous dispersion, vacuum degassing, filtering and filling on the base material after the homogeneous grinding to obtain the sample of the comparative example 2.
The following main technical criteria were tested on the sample of comparative example 2, and the results are shown in table 6 below:
TABLE 6 main technical index test results of the sample of comparative example 2
| Serial number | Inspection item | Unit of | Standard requirements | Test results |
| 1 | Appearance of the product | / | Homogeneous, free of extraneous matter | Qualified |
| 2 | Cone penetration (-40 ℃ C.) | 1/10mm | ≥230 | 285 |
| 3 | Oil separating (80 ℃, 24h) | ％ | ≤0.5 | 0 |
| 4 | High temperature stability at 80 deg.C | 24h | —— | By passing |
| 5 | Oxidative induction period (190 ℃ C.) | min | ≥20 | 60 |
| 6 | Yield stress (25 ℃ C.) | pa | —— | 45 |
| 7 | PBT weight ratio (85 ℃, 45X24 h) | ％ | ≤3 | 0.68 |
| 8 | Optical fiber weight ratio (85 ℃, 30X24 h) | ％ | —— | 0.31 |
Comparative example 3
(1) Putting 879 g of GTL base oil into a reaction kettle, putting 65 g of measured SEP thermoplastic rubber and 25 g of SV260 viscosity index improver into the reaction kettle, heating while stirring, adding 5g of measured antioxidant when the temperature is increased to 160 ℃, stirring for 3-5 hours at constant temperature until the SEP thermoplastic rubber and the SV260 viscosity index improver are completely dissolved in the GTL base oil to form a master batch, then moving the master batch out of the reaction kettle, and cooling to below 60 ℃ for later use;
(2) adding the cooled master batch into a stirring kettle, slowly adding 20 g of the measured multi-walled carbon nanotubes into the stirring kettle, sequentially stirring while adding, stirring for 1-2 hours after the multi-walled carbon nanotubes are completely soaked in the master batch, adding 6 g of PEG400 type structure stabilizer, and continuously stirring for 1-2 hours to form a base material;
(3) and (3) carrying out high-pressure homogenizing grinding on the base material by a high-pressure homogenizing pump, wherein the homogenizing pressure is controlled at 30 MPa.
(4) And (3) carrying out homogeneous dispersion, vacuum degassing, filtering and filling on the base material after the homogeneous grinding to obtain the sample of the comparative example 3.
The following main technical criteria were tested on the sample of comparative example 3, and the results are shown in table 7 below:
TABLE 7 main technical index test results of the sample of comparative example 3
| Serial number | Inspection item | Unit of | Standard requirements | Test results |
| 1 | Appearance of the product | / | Homogeneous, free of extraneous matter | Qualified |
| 2 | Cone penetration (-40 ℃ C.) | 1/10mm | ≥230 | 280 |
| 3 | Oil separating (80 ℃, 24h) | ％ | ≤0.5 | 0 |
| 4 | High temperature stability at 80 deg.C | 24h | —— | By passing |
| 5 | Oxidative induction period (190 ℃ C.) | min | ≥20 | 60 |
| 6 | Yield stress (25 ℃ C.) | pa | —— | 57 |
| 7 | PBT weight ratio (85 ℃, 45X24 h) | ％ | ≤3 | 0.69 |
| 8 | Optical fiber weight ratio (85 ℃, 30X24 h) | ％ | —— | 0.32 |
By combining the analysis of examples 1 to 4 and comparative examples 1 to 3, as can be seen by comparing example 1 with comparative example 1, in the case where the control variables are such that the GTL base oil is only adjusted to the hydrogenated white oil currently used in the industry, the cone penetration (-40 ℃) of comparative example 1 is 2401/10 mm, which is significantly lower than 2801/10 mm of example 1, indicating that the stability under low temperature environment is far less than that of the technical solution of the present invention, meanwhile, the weight ratio of the PBT in the embodiment 1 (85 ℃, 45 multiplied by 24h) is 0.7 percent, the weight ratio of the optical fiber (85 ℃, 30 multiplied by 24h) is 0.3 percent, the PBT weight gain ratio (85 ℃, 45X24 h) of the Bili 1 is 2.1 percent, the optical fiber weight gain ratio (85 ℃, 30X24 h) is 0.85 percent, which is far higher than the test result of the example 1, and is very close to the minimum requirement in the industry, and the reliability is far lower than that of the example 1; by comparing example 2, comparative example 2 and comparative example 3 respectively, the yield stress (25 ℃) of example 2 is 68pa, the yield stress (25 ℃) of comparative example 2 is 45pa, the yield stress (25 ℃) of comparative example 3 is 57pa, comparative example 2 is different from example 2 in that carbon nanotubes are not used and a three-dimensional network structure is not formed due to vacuum centrifugal operation, comparative example 3 is different from example 2 in that a three-dimensional network structure is not formed due to vacuum centrifugal operation, and comparative example 2 is different from comparative example 3 in that carbon nanotubes are not added, so that the addition of carbon nanotubes has the effect of toughening and strengthening on the technical scheme of the invention, while the vacuum centrifugal operation further strengthens the strengthening effect, the combined use of carbon nanotubes and vacuum toughening and centrifugal operation strengthens and ensures the toughening and strengthening effect, and the yield stress of example 2 is much higher than that of comparative example 2 and comparative example 3, therefore, the optical fiber filling paste provided by the invention can be used for sufficiently protecting optical cables and optical fibers, reducing the loss of the optical fibers and prolonging the service life of the optical fibers.
The optical fiber filling paste with ultralow loss for the optical fiber does not need to be heated when the sleeve is filled, and belongs to cold application normal-temperature filling paste. The high-temperature-resistant optical fiber cable sheath has the characteristics that the paste has excellent high-low temperature performance and yield stress, the stability of paste colloid is good, the structure shear is stable, the strength and the toughness are certain, and the compatibility with an optical fiber sheath material and a tight-sleeve material is very excellent. It can make the optical fiber in the loose tube and the cable core in the cable be in the most free and stress-free state all the time, thus reducing the microbending loss of the optical fiber and the stress corrosion of the optical fiber under the action of stress, moisture and humidity. When the optical fiber filling paste is stressed (such as carrying and hoisting of an optical cable), the optical fiber is fixed in a solid state; when the stress is above a critical value (e.g., bending, jerking, etc.), the paste flows and the viscosity drops rapidly, so that the fiber can be stressed while releasing the stress without bending. Moreover, because the thermodynamic phase of the optical fiber filling paste of the present invention tends to be solid, the optical fiber filling paste of the present invention gradually returns to high viscosity after the optical fiber is free to fix the optical fiber; the transmission quality of the optical cable is greatly improved. The stress mainly plays a role in protecting the optical fiber in time once the optical fiber is subjected to external force, and the optical fiber cannot generate any signal transmission in a free state. When the common fiber paste is subjected to the stress, the optical fiber is simultaneously subjected to the stress, so that the optical fiber is in a local stress state for a long time, large bending and micro bending loss are generated, and stress corrosion is generated under the action of moisture. In general, the additive loss is reduced by 50% or more and the additional loss in cabling is reduced by 20% or more when the optical fiber filling paste of the present invention is used, and in a single-mode optical fiber system having a wavelength of 1.55 μm, the transmission link can be increased by 10Km, that is, by 12%, and if various benefits (such as reduction in modal dispersion) due to the reduction in the stress applied to the optical fiber during use are added, the quality of optical communication is further improved. More importantly, the protection of the optical fiber filling paste of the present invention against stress and moisture of the optical fiber in the loose tube actually ensures the service life of the optical fiber, and those skilled in the art know that randomly distributed cracks in the optical fiber, particularly surface microcracks formed during rod making and wire drawing, are the fundamental reasons affecting the strength of the optical fiber. During the process of laying and using the optical cable, the surface cracks of the optical fiber can continue to expand under the action of stress and moisture, so that the strength of the optical fiber is reduced, and finally, the optical fiber is broken, namely, the static fatigue process of the optical fiber. Thus, cracks in the optical fiber, especially on the surface of the optical fiber, are intrinsic factors in the fiber fracture, while stress and moisture are extrinsic factors that promote crack propagation and ultimately lead to fiber fracture. Therefore, the optical fiber is protected by the optical fiber filling paste in the loose tube, the invasion of stress and moisture to the optical fiber is basically inhibited, the static fatigue of the optical fiber is greatly reduced, the service life of the optical fiber is effectively ensured, and the safe operation of the optical cable under various environments and climatic conditions is ensured.
The above embodiments are provided only for illustrating the present invention and not for limiting the present invention, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the present invention, and therefore all equivalent technical solutions should also fall within the scope of the present invention, and should be defined by the claims.
Claims (7)
1. The optical fiber filling paste is characterized by comprising the following components in percentage by weight:
the sum of the weight percentage contents of the components is 100 percent;
the carbon nano-tube is a multi-wall carbon nano-tube.
2. The ultra-low loss optical fiber filling paste of claim 1 wherein said polymer elastomer is an SEP thermoplastic.
3. The optical fiber filling paste as claimed in claim 1, wherein the viscosity index improver is SV 260.
4. The ultra-low loss optical fiber filling paste of claim 1, wherein said structure stabilizer is polyethylene glycol.
5. The ultra-low loss optical fiber filling paste for optical fiber according to claim 1, wherein the antioxidant is a composite high temperature liquid antioxidant.
6. A method for preparing the ultra-low loss optical fiber filling paste for optical fiber according to claim 1, comprising the steps of:
the method comprises the following steps: preparing raw materials according to the following components in percentage by weight:
the sum of the weight percentage contents of the components is 100 percent;
the carbon nano tube is a multi-wall carbon nano tube;
step two: adding the GTL base oil, the polymer synthetic rubber and the viscosity index improver prepared in the step one into a reaction kettle, heating while stirring, adding the antioxidant prepared in the step one into the reaction kettle when the temperature is raised to 160 ℃, stirring at constant temperature for 3-5 hours until the polymer synthetic rubber and the viscosity index improver are completely dissolved in the GTL base oil to form a master batch, transferring the master batch out of the reaction kettle, and cooling the master batch to be lower than 60 ℃ for later use;
step three: adding the cooled master batch in the second step into a stirring kettle, slowly adding the carbon nano tubes prepared in the first step into the stirring kettle, continuously stirring for 1-2 hours after the carbon nano tubes are completely soaked in the master batch, then adding the structure stabilizer prepared in the first step, and continuously stirring for 1-2 hours to form a base material;
step four: carrying out high-pressure homogenizing grinding on the base material in the third step by a high-pressure homogenizing pump, wherein the homogenizing pressure is controlled to be about 25-35 MPa;
step five: and C, carrying out homogenizing dispersion, vacuum degassing, vacuum centrifugation, filtration and filling on the base material subjected to high-pressure homogenizing grinding in the fourth step.
7. The method as claimed in claim 6, wherein the centrifugation speed is 2000-3500 rpm and the vacuum pressure is-0.07 to-0.1 MPa when the vacuum centrifugation is performed in step five.
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Application publication date: 20201023 |