CN107880557B - High-expansion-ratio silicone rubber cold-shrink tube and preparation method and application thereof - Google Patents
High-expansion-ratio silicone rubber cold-shrink tube and preparation method and application thereof Download PDFInfo
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- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
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Abstract
The invention relates to a silicone rubber cold-shrink tube with high expansion ratio, a preparation method and an application thereof, wherein the silicone rubber cold-shrink tube is prepared from the following components in parts by mass: 80-100 parts of organopolysiloxane, 30-50 parts of reinforcing filler, 3-10 parts of organic silicon resin, 3-15 parts of structural control agent, 0.05-0.8 part of catalyst, 0.5-5 parts of cross-linking agent, 1-5 parts of chain extender and 0.05-0.4 part of reaction inhibitor. The silicone rubber cold-shrink tube prepared by the formula provided by the invention has good mechanical property, can be directly expanded for 5 times for use, does not need a multilayer structure or compounding of multiple materials, is simple to use, has good retraction performance, and can meet the moisture-proof sealing requirement of a novel antenna feeder system with overlarge difference of the thickness parts of the connector.
Description
Technical Field
The invention relates to the field of chemical materials, in particular to a silicone rubber cold-shrink tube with high expansion rate and a preparation method and application thereof.
Background
With the continuous development of 4G communication technology, the construction of 4G networks is accelerated by large mobile operators, and the number of base stations to be built increases continuously. With the continuous maturation of the 5G technology, the number of newly built base stations is expected to increase greatly in the future. The reliability of the base station system is related to the safe and stable operation of the communication network. The reliability of the antenna feeder accounts for 30% -50% of the reliability of the whole base station system, and one of the most common problems of the antenna feeder system is that the antenna feeder connector is affected with damp and water due to poor sealing, so that standing-wave ratio alarm is caused, and normal operation of the base station is influenced.
The sealing methods commonly used for the antenna feeder connector at present include a waterproof adhesive tape, a waterproof box, a heat shrink tube, a cold shrink tube and the like. The waterproof adhesive tape needs to be wound during construction, is troublesome to construct and maintain, and has poor waterproof performance and service life; the waterproof box is suitable for antenna feeder systems with larger installation intervals and is not suitable for base station systems which are more and more compact; the heat shrink tube needs to use an electric heating device or open fire when being installed, is poor in safety, cannot breathe with the cable body at the same time, and is poor in waterproof effect. The cold shrink tube does not need to use a heating device during installation, is simple and convenient to operate and use, has long service life, can breathe with the cable body simultaneously, and has a good waterproof effect. The cold-shrink tube made of the silicone rubber material has the advantages of excellent aging resistance, long-term use in outdoor environment, good waterproof and hydrophobic properties and the like, and is more and more widely applied. Patent CN101544834B discloses a preparation method and application of a cold-shrink type power silicone rubber sleeve, which is applied to the terminal connection of various cables in a power cable line, and forms a power transmission network together with the cables. However, the expansion rate of the cold-shrinkage power silicone rubber sleeve applied to the connection of the cable terminal is generally within 3 times, and the performance requirement of 5 times of expansion cannot be met, and meanwhile, the thermal aging shrinkage performance cannot meet the waterproof requirement of the non-equal-diameter sealed thin end. Patent CN 204886114U discloses a high multiplying power silicon rubber cold-shrinkable tube, and this high multiplying power silicon rubber cold-shrinkable tube is through increasing first sheath and second sheath outside the silicon rubber and supply the not enough of silicon rubber performance, and the structure is complicated, and it is loaded down with trivial details to expand the technology in advance, is unfavorable for the enterprise to improve production efficiency and reduction in production cost. Patent CN103595010B discloses an insulation sealing method for non-equal diameter objects, which can solve the insulation sealing problem for non-equal diameter objects, and make both the thick end and the thin end well sealed. The method adopts two specifications of cold-shrinkable tubes, the first cold-shrinkable tube is firstly shrunk on the thin end of the non-equal-diameter object to make the thin end close to the thick end, and then the second cold-shrinkable tube is shrunk on the thick end and the first cold-shrinkable tube. The method uses cold-shrink tubes with two specifications, so that the installation is troublesome and the cost is obviously increased. Patent CN 205791324U discloses an ethylene propylene rubber double-layer cold shrinkage pipe with a built-in silicone tube, wherein the cold shrinkage pipe can be expanded to about 4.5 times and can be used for sealing connection of communication and other wired coaxial cables. However, the ethylene propylene rubber pipe outside the inner silica gel pipe is adopted, so that the extrusion production difficulty is high, the expansion is difficult, and meanwhile, the low-temperature resistance and the service life of the ethylene propylene rubber layer on the outer layer are inferior to those of the inner silica gel pipe, so that the failure of the ethylene propylene rubber layer is accelerated when the ethylene propylene rubber pipe is used in a long-term low-temperature environment, and the whole service life is influenced.
Therefore, the development of a silicone rubber cold-shrink tube with high expansion rate, simple process, high production efficiency and low cost and a preparation method thereof are urgently needed.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the silicone rubber cold-shrink tube with high expansion rate, which has better mechanical property, can be directly expanded for 5 times for use, does not need a multilayer structure or compounding of multiple materials and has good retraction performance.
The invention also aims to provide a preparation method of the silicone rubber cold-shrinkable tube with high expansion ratio.
The invention also aims to provide the application of the high-expansion-ratio silicone rubber cold-shrinkable tube in waterproof sealing of communication base stations and cable television cables.
In order to achieve the purpose, the invention adopts the following technical scheme:
the silicone rubber cold-shrinkable tube with the high expansion ratio is prepared from the following components in parts by mass:
80-100 parts of organopolysiloxane, 30-50 parts of reinforcing filler, 3-10 parts of organic silicon resin, 3-15 parts of structural control agent, 0.05-0.8 part of catalyst, 0.5-5 parts of cross-linking agent, 1-5 parts of chain extender and 0.05-0.4 part of reaction inhibitor;
wherein the structural formula of the organic silicon resin is as follows:
[(CH3)3SiO1/2]e[(CH2＝CH)(CH3)2SiO1/2]f[(CH3)2SiO2/2]g[SiO4/2]
in the formula, the value of e is 0.2-0.6, f is 0.1-0.4, and g is 0.2-0.4;
the structural formula of the chain extender is as follows:
in the formula, the value of h is 11-88.
According to the invention, the organic silicon resin with a specific structure is selected, and the organic silicon resin is provided with the D chain link, so that the flexibility and the ductility of the product can be improved, the tensile strength and the tearing strength of the prepared silicone rubber cold-shrinkable tube can be further improved, the retraction performance after installation can be ensured, and the requirements of sealing and water proofing can be met. In addition, the invention further increases the length of the main chain by adding the chain extender to participate in crosslinking, thereby improving the elongation at break of the product. Through the selection of the organic silicon resin with a specific structure and the chain extender, the prepared silicone rubber cold-shrinkable tube can meet the performance requirement of 5 times expansion.
The silicone rubber cold-shrink tube prepared by the formula provided by the invention has good mechanical property, can be directly expanded by 5 times for use, does not need a multilayer structure or compounding of multiple materials, is simple to use, has good retraction performance, and can meet the moisture-proof sealing requirement of a coaxial cable with an overlarge difference between the thickness of a connector and the thickness of a connector.
Preferably, the silicone rubber cold-shrinkable tube is prepared from the following components in parts by mass:
90-100 parts of organopolysiloxane, 35-45 parts of reinforcing filler, 3-8 parts of organic silicon resin, 5-10 parts of structural control agent, 0.1-0.5 part of catalyst, 0.8-4 parts of cross-linking agent, 1.5-4 parts of chain extender and 0.1-0.3 part of reaction inhibitor.
Preferably, in the structural formula of the organic silicon resin, the value of e is 0.3-0.5, the value of f is 0.2-0.3, and the value of g is 0.3-0.4.
Preferably, in the structural formula of the organic silicon resin, the value of e is 0.4, f is 0.2, and g is 0.3.
Preferably, in the structural formula of the chain extender, the value of h is 44-77.
Preferably, in the structural formula of the chain extender, the value of h is 55.
Preferably, the organopolysiloxane has the following structural formula:
wherein the value of a is 6000-10700, and the value of b is 8-50; r1And R2All are C2-C4 alkenyl.
More preferably, the value of a is 8200-9800, and the value of b is 20-30.
Preferably, the reinforcing filler has a BET specific surface area of 150-380 m2(ii) a bulk density of 40 to 200kg/m3The fumed silica of (3), the fumed silica having undergone a hydrophobization treatment, or both.
Preferably, the cross-linking agent has the following structural formula:
in the formula, c is 15-50, d is 6-100, R3 is methyl or hydrogen radical, and R4 is hydrogen radical.
Preferably, the structural control agent is one or more of hexamethyldisilazane, octamethylcyclotetrasiloxane, micromolecule hydroxyl silicone oil, methyltrisilazane, tetramethyldivinyldisilazane, trimethylchlorosilane, dimethyldichlorosilane or methyltrichlorosilane.
Preferably, the reaction catalyst is one or more of a platinum catalyst, a palladium catalyst and a rhodium catalyst; wherein the platinum catalyst can be a reaction product of chloroplatinic acid and hydroxyl alcohol, a complex of chloroplatinic acid and olefin, platinum tetrachloride, chloroplatinic acid or platinum diacetylacetate.
Preferably, the reaction inhibitor is one or more of 1-ethynyl-1-cyclohexanol, methylbutynol, 3, 5-dimethyl-1-hexynyl-3-ol, vinyl ring body, fumarate or maleate.
The preparation method of the high-expansion-ratio silicone rubber cold-shrinkable tube comprises the following steps:
s1: adding the organopolysiloxane, the reinforcing filler, the organic silicon resin and the structural control machine into a kneading machine for kneading, then heating for heat treatment, and vacuumizing to obtain a sizing material A;
s2: placing the rubber material A in an open mill, adding a catalyst, a cross-linking agent, a chain extender and a reaction inhibitor for mixing, and filtering to obtain a rubber material B after mixing is finished;
s3: feeding the rubber material B into a screw extruder for continuous extrusion, and forming through a high-temperature pre-vulcanization furnace and a post-vulcanization drying tunnel to obtain the silicone rubber cold-shrinkable tube.
Preferably, in S1, the raw materials are kneaded in a kneader for 1-3 h; the parameters of the heat treatment are as follows: the temperature is 100-150 ℃, and the heat treatment time is 1-3 h; the vacuumizing time is 0.5-3 h, and the vacuum degree is-0.085 to-0.1 MPa.
Preferably, in S2, the mixing time is 10-20 min; the open mill adopts a water cooling mode, and the temperature of the materials is controlled to be not higher than 50 ℃.
Preferably, in S3, the screw extruder is cooled by water, the temperature of the high-temperature pre-vulcanization furnace is 300-800 ℃, and the temperature of the post-vulcanization drying tunnel is 120-350 ℃.
The invention also protects the application of the high-expansion-ratio silicone rubber cold-shrinkable tube in waterproof sealing of communication base stations and cable television cables.
Compared with the prior art, the invention has the following beneficial effects:
tests prove that the Shore hardness of the silicone rubber cold-shrinkable tube is 35-42A, the tensile strength is more than or equal to 10.0MPa, the elongation at break is more than or equal to 850%, the tearing strength is more than or equal to 35.0KN/mm, and the permanent deformation at break is less than or equal to 4.8%. The expansion rate of the silicone rubber cold-shrinkable tube provided by the invention can reach 5 times, and the silicone rubber cold-shrinkable tube can be applied to waterproof sealing of communication base stations and other exposed coaxial cable joints. Because the expansion rate of the silicon rubber cold-shrinkable tube is high, the retraction ratio is large after the support bracket is pulled out, and the waterproof sealing device is particularly suitable for waterproof sealing of coaxial cables with large thickness difference of the connection part (the diameter of the thick end is larger than or equal to 2.5: 1).
Detailed Description
The present invention is further illustrated by the following specific examples, which are not intended to limit the invention in any way. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Unless otherwise indicated, reagents and materials used in the present invention are commercially available.
Example 1
The silicone rubber cold-shrinkable tube with the high expansion ratio is prepared from the following components in parts by mass:
80kg of organopolysiloxane, 30kg of reinforcing filler, 3kg of organic silicon resin, 3kg of structural control agent, 0.05kg of catalyst, 0.5kg of cross-linking agent, 1kg of chain extender and 0.05kg of reaction inhibitor;
wherein the structural formula of the organic silicon resin is as follows:
[(CH3)3SiO1/2]e[(CH2＝CH)(CH3)2SiO1/2]f[(CH3)2SiO2/2]g[SiO4/2]
in the formula, the value of e is 0.2, f is 0.1, and g is 0.2;
the structural formula of the chain extender is as follows:
wherein h is 11.
The preparation method of the high-expansion-ratio silicone rubber cold-shrinkable tube comprises the following steps:
(1) adding organopolysiloxane, reinforcing filler, organic silicon resin and a structural control agent into a kneading machine, kneading for 1-3 h, heating to 100-150 ℃, performing heat treatment for 1-3 h, vacuumizing for 0.5-3 h, and obtaining a sizing material A under the vacuum degree of-0.085-0.1 MPa;
(2) and adding a catalyst, a cross-linking agent, a chain extender and a reaction inhibitor into the rubber material A on an open mill, and mixing for 10-20 min. The open mill adopts a water cooling mode, and the material temperature is controlled to be not higher than 50 ℃. After mixing, filtering to obtain a rubber material B;
(3) and continuously extruding the rubber material B by feeding the rubber material B into a screw extruder, and forming the rubber material B by a high-temperature pre-vulcanization furnace and a post-vulcanization drying tunnel after extrusion. The screw extruder is cooled by water, the temperature of a high-temperature pre-vulcanization furnace is 300-800 ℃, and the temperature of a post-vulcanization drying tunnel is 120-350 ℃.
Example 2
The silicone rubber cold-shrinkable tube with the high expansion ratio is prepared from the following components in parts by mass:
100kg of organopolysiloxane, 50kg of reinforcing filler, 10kg of silicone resin, 15kg of structural control agent, 0.8kg of catalyst, 5kg of cross-linking agent, 5kg of chain extender and 0.4kg of reaction inhibitor;
wherein the structural formula of the organic silicon resin is as follows:
[(CH3)3SiO1/2]e[(CH2＝CH)(CH3)2SiO1/2]f[(CH3)2SiO2/2]g[SiO4/2]in the formula, the value of e is 0.6, f is 0.4, and g is 0.4;
the structural formula of the chain extender is as follows:
wherein h is 88.
The preparation method of the silicone rubber cold shrinkable tube provided in this example is the same as that of example 1.
Example 3
The silicone rubber cold-shrinkable tube with the high expansion ratio is prepared from the following components in parts by mass:
90kg of organopolysiloxane, 40kg of reinforcing filler, 6kg of organic silicon resin, 9kg of structural control agent, 0.5kg of catalyst, 3.5kg of cross-linking agent, 4.0kg of chain extender and 0.3kg of reaction inhibitor;
wherein the structural formula of the organic silicon resin is as follows:
[(CH3)3SiO1/2]e[(CH2＝CH)(CH3)2SiO1/2]f[(CH3)2SiO2/2]g[SiO4/2]in the formula, the value of e is 0.4, f is 0.2, and g is 0.3;
the structural formula of the chain extender is as follows: wherein h is 55.
The preparation method of the silicone rubber cold shrinkable tube provided in this example is the same as that of example 1.
Example 4
The silicone rubber cold-shrinkable tube with the high expansion ratio is prepared from the following components in parts by mass:
100kg of organopolysiloxane, 30kg of reinforcing filler, 8kg of organic silicon resin, 9kg of structural control agent, 0.3kg of catalyst, 3.0kg of cross-linking agent, 2.5kg of chain extender and 0.1kg of reaction inhibitor;
wherein the structural formula of the organic silicon resin is as follows:
[(CH3)3SiO1/2]e[(CH2＝CH)(CH3)2SiO1/2]f[(CH3)2SiO2/2]g[SiO4/2]
in the formula, the value of e is 0.3, f is 0.2, and g is 0.4;
the structural formula of the chain extender is as follows:
wherein h is 44.
The preparation method of the silicone rubber cold shrinkable tube provided in this example is the same as that of example 1.
Comparative example 1
The components, the amount and the preparation method of the silicone rubber cold-shrinkable tube provided by the comparative example are the same as those of example 1, except that no silicone resin is added in the comparative example.
Comparative example 2
The components, the using amount and the preparation method of the silicone rubber cold-shrinkable tube provided by the comparative example are the same as those of example 1, and the difference is that no chain extender is added in the comparative example.
Comparative example 3
The components, the using amount and the preparation method of the silicone rubber cold-shrinkable tube provided by the comparative example are the same as those of example 1, and the difference is that the structural formula of the silicone resin selected by the comparative example is as follows:
[(CH3)3SiO1/2]e[(CH2＝CH)(CH3)2SiO1/2]f[SiO4/2]g
in the formula, the value of e is 0.2, f is 0.1, and g is 0.2.
Comparative example 4
The components, the using amount and the preparation method of the silicone rubber cold-shrinkable tube provided by the comparative example are the same as those of example 1, and the difference is that the structural formula of the selected chain extender is as follows:
wherein m is 800.
The properties of the silicone rubber cold-shrinkable tubes prepared in the above examples and comparative examples were measured by the following methods, and the results are shown in table 1 below.
TABLE 1 Performance test of Silicone rubber Cold shrink tubes prepared in examples 1 to 4 and comparative examples 1 to 4
From the experimental data of the above examples and comparative examples, it can be seen that the formulation performance within the limits of the present invention can meet the 5-fold expansion requirement. Comparative example 1 no silicone resin was added, and the tensile strength, elongation at break and tear strength were all low, only meeting the requirement of 4 times expansion; comparative example 2 no chain extender was added, the elongation at break was low and only 3 times the extension requirement was met; the comparative example 3 is added with other organic silicone resin, although the tensile strength and the tearing strength can meet the requirements, the elongation at break is obviously smaller, and the requirement of 3 times of expansion can be met; the comparative example 4 selects the chain extender with other configurations, the chain extension effect is not obvious, the improvement of the elongation at break is not obviously helped, and the requirement of 5 times of expansion cannot be met.
Claims (8)
1. The high-expansion-ratio silicone rubber cold-shrinkable tube is characterized by being prepared from the following components in parts by mass:
80-100 parts of organopolysiloxane, 30-50 parts of reinforcing filler, 3-10 parts of organic silicon resin, 3-15 parts of a structural control agent, 0.05-0.8 part of a catalyst, 0.5-5 parts of a cross-linking agent, 1-5 parts of a chain extender and 0.05-0.4 part of a reaction inhibitor;
wherein the structural formula of the organic silicon resin is as follows:
[(CH3)3SiO1/2]e[(CH2＝CH)(CH3)2SiO1/2]f[(CH3)2SiO2/2]g[SiO4/2]in the formula, the value of e is 0.2-0.6, f is 0.1-0.4, and g is 0.2-0.4;
the structural formula of the chain extender is as follows:
in the formula, the value of h is 11-88;
the structural formula of the organopolysiloxane is as follows:
wherein the value of a is 6000-10700, and the value of b is 8-50; r1And R2All are C2-C4 alkenyl;
the structural formula of the cross-linking agent is as follows:
in the formula, the value of c is 15-50, the value of d is 6-100, R3 is methyl or hydrogen radical, and R4 is hydrogen radical.
2. The silicone rubber cold shrink tube with high expansion ratio of claim 1, wherein the silicone rubber cold shrink tube is prepared from the following components in parts by mass:
90-100 parts of organopolysiloxane, 35-45 parts of reinforcing filler, 3-8 parts of organic silicon resin, 5-10 parts of structural control agent, 0.1-0.5 part of catalyst, 0.8-4 parts of cross-linking agent, 1.5-4 parts of chain extender and 0.1-0.3 part of reaction inhibitor.
3. The silicone rubber cold shrink tube with high expansion ratio as claimed in claim 1, wherein in the structural formula of the silicone resin, the value of e is 0.3-0.5, the value of f is 0.2-0.3, and the value of g is 0.3-0.4.
4. The silicone rubber cold shrink tube with high expansion ratio of claim 3, wherein in the structural formula of the silicone resin, the value of e is 0.4, f is 0.2, and g is 0.3.
5. The silicone rubber cold shrink tube with high expansion ratio as claimed in claim 1, wherein in the structural formula of the chain extender, the value of h is 44-77.
6. The silicone rubber cold shrink tube with high expansion ratio of claim 5, wherein in the structural formula of the chain extender, the value of h is 55.
7. The method for preparing the silicone rubber cold-shrinkable tube with high expansion ratio of any one of claims 1 to 6, which is characterized by comprising the following steps:
s1: adding the organopolysiloxane, the reinforcing filler, the organic silicon resin and the structural control agent into a kneading machine for kneading, then heating for heat treatment, and vacuumizing to obtain a sizing material A;
s2: placing the rubber material A in an open mill, adding a catalyst, a cross-linking agent, a chain extender and a reaction inhibitor for mixing, and filtering to obtain a rubber material B after mixing is finished;
s3: feeding the rubber material B into a screw extruder for continuous extrusion, and forming through a high-temperature pre-vulcanization furnace and a post-vulcanization drying tunnel to obtain the silicone rubber cold-shrinkable tube.
8. The use of the high expansion ratio silicone rubber cold-shrinkable tube according to any one of claims 1 to 6 in waterproof sealing of communication base stations and cable television cables.
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