CN110452444B - Crosslinked polyethylene composite material with super-hydrophobic characteristic, preparation method and application - Google Patents
Crosslinked polyethylene composite material with super-hydrophobic characteristic, preparation method and application Download PDFInfo
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Abstract
The invention discloses a crosslinked polyethylene composite material with super-hydrophobic characteristics, a preparation method and application thereof. The crosslinked polyethylene composite material of the invention is filled with mesoporous nano-silica of which the surface is modified with fluorine-containing functional molecules, thereby realizing the super-hydrophobic characteristic. The crosslinked polyethylene composite material provided by the invention can be used as a main insulating material of a cable, effectively inhibits the defects of cable water tree degradation and the like caused by water vapor, moisture and other factors, and greatly improves the operation safety and stability of the cable.
Description
Technical Field
The invention relates to the technical field of insulating composite materials, in particular to a crosslinked polyethylene composite material with super-hydrophobic characteristics, a preparation method and application thereof.
Background
With the rapid development of economy and the upgrading and reconstruction of power grids in China, power cables are widely applied to urban power distribution networks due to the advantages of small occupied area, easiness in laying, simplicity and convenience in maintenance, excellent insulating property and the like. The cross-linked polyethylene (XLPE) cable is widely applied to urban power distribution networks due to excellent mechanical property, electrical property and heat-resistant property, and the safe, reliable and stable operation of the cable has important significance for urban development.
At present, power cables are mostly buried underground in urban power transmission. In the moist environment of underground, the cable insulating layer is inevitable to suffer the corruption and the invasion of moisture, under the long-term effect of electric field, very easily forms the water tree defect and causes the insulation degradation, and the water tree grows to certain length and can initiate permanent electric tree defect at the pointed end promptly to lead to cable insulation breakdown and then take place power transmission trouble in the short time, seriously influence the life and the operational reliability of cable.
Disclosure of Invention
The invention aims to provide a crosslinked polyethylene composite material with a super-hydrophobic characteristic, so as to solve the problems that the existing crosslinked polyethylene cable insulating material is easy to damp and has a poor hydrophobic effect.
In addition, the invention also provides a preparation method and application of the crosslinked polyethylene composite material with the super-hydrophobic characteristic.
The invention is realized by the following technical scheme:
the crosslinked polyethylene composite material with super-hydrophobic characteristic takes crosslinked polyethylene as a matrix and takes mesoporous nano-silica with fluorine-containing functional molecules modified on the surface as a filler.
The applicant found through experiments that: the hydrophobic property of the material can be effectively improved by a certain physical and chemical method, so that the problem of cable moisture can be solved by improving the hydrophobicity of the crosslinked polyethylene matrix.
The hydrophobicity of the material is determined by the chemical composition and the microstructure of the material, and the invention utilizes the nano mesoporous silicon dioxide (mSiO) with fluorine-containing functional molecules modified on the surface2-C8F13H4) The mesoporous silicon dioxide is compounded with cross-linked polyethylene (XLPE), the multi-gap characteristic of the mesoporous silicon dioxide is beneficial to improving the contact area between the filler and the polymer matrix, and the fluorine atoms can form intermolecular hydrogen bonds with the cross-linked polyethylene, thereby obviously enhancing the compoundThe interface effect of the material finally prepares the material with the super-hydrophobic characteristic (the contact angle is larger than 150 degrees) and the insulating characteristic (the breakdown strength)>35kV/mm, volume resistivity>1015Ω · m) is used as the crosslinking polyethylene composite material.
Compared with the existing crosslinked polyethylene material, the contact angle of the composite material provided by the invention is obviously improved, and the composite material has good insulating property, and the crosslinked polyethylene composite material provided by the invention has a high contact angle (larger than 150 degrees), a dielectric constant of less than 2.5 and a breakdown field strength of more than 35 kV/mm.
The invention relates to mesoporous nano silicon dioxide (mSiO) with the surface modified with fluorine-containing functional molecules2-C8F13H4) The cable insulation material not only has porosity, but also has strong electronegativity of fluorine atoms, enhances the interface effect with crosslinked polyethylene by establishing intermolecular hydrogen bonds, reduces the surface free energy of the composite material, realizes the super-hydrophobic characteristic, and solves the problems that the existing crosslinked polyethylene cable insulation material is easy to damp and has poor hydrophobic effect.
Further, the mass percentages of the filler and the matrix are as follows: 19% -32.8%: 81 to 67.2 percent.
The applicant found through experiments that: when the filler content is less than 19%, the hydrophobic property of the resulting composite material may not be satisfactory, and when the filler content exceeds 32.8%, the processing property, mechanical strength, and puncture strength of the composite material may be reduced.
Further, the crosslinked polyethylene is low-density polyethylene, and the density of the low-density polyethylene is 0.912-0.924 g/cm3The molecular weight is 146500-179500.
The molecular weight and density of the low-density polyethylene are selected based on the most common LDPE in the current cable production process, and the aim is to enable the matrix of the obtained composite material to be close to XLPE in actual production, so that the effects of surface functional molecules and groups of the nanoparticles in the performance regulation of the composite material can be reflected. )
Further, the modifier for modifying the mesoporous nano-silica is triethoxy-1H, 1H,2H, 2H-tridecafluoro-n-octylsilane.
triethoxy-1H, 1H,2H, 2H-tridecafluoro-n-octyl silane is selected as a surface functional modification molecule, and the aim is to (1) improve the dispersibility of nanoparticles in an XLPE matrix; (2) providing enough fluorine atoms to enhance the interfacial action and the interfacial compatibility between the XLPE and the nano-particles by forming hydrogen bonds; (3) fully utilizes the hydrophobic property of the fluorine-containing group.
Further, the mass ratio of the modifier to the mesoporous nano-silica is as follows: 0.2-0.4: 1.
the function between the modifier and the mesoporous silica is formed by the covalent bond between hydroxyl groups on the surface of the mesoporous silica and modifier molecules. The hydroxyl content of the surface of the mesoporous silica is generally less than 10%, in order to enable the surface modification to be more thorough, the content of the modifier is preferably 2-4 times of the hydroxyl content, and due to the limited reaction sites, raw materials can only be wasted at a higher proportion.
Furthermore, the average particle diameter of the mesoporous nano-silica is 50-100 nm, and the average pore diameter is 0.6-5 nm.
A method for preparing a cross-linked polyethylene composite material with super-hydrophobic characteristics comprises the following steps:
1) and prepolymer blending: mixing crosslinked polyethylene and mesoporous nano-silica, and then melting and blending at 105-110 ℃ to obtain a blending prepolymer compound with filler particles uniformly dispersed in the crosslinked polyethylene;
2) blending the prepolymer and the cross-linking agent: melting and blending the blending prepolymer compound and dicumyl peroxide at 108-110 ℃ to obtain a ternary blending compound;
3) and hot-press forming: hot-pressing and molding the ternary blend compound under the conditions of 13-15 Mpa and 108-115 ℃ by adopting a flat vulcanizing machine to prepare a sample;
4) and vulcanization crosslinking: and crosslinking the sample for 30-50min at 168-174 ℃ and 13-16MPa by adopting a flat vulcanizing machine to obtain the crosslinked polyethylene composite material.
The specific preparation process of the fluorine-containing functional molecule modified mesoporous nano-silica comprises the following steps:
1) ultrasonically dispersing triethoxy-1H, 1H,2H, 2H-tridecafluoro-n-octylsilane and mesoporous nano-silica in an organic solvent according to a certain proportion to obtain a uniformly dispersed solution, wherein the organic solvent is anhydrous toluene (the water content is: 3-28 ppm), the ultrasonic power is 80-100W, and the frequency is 40-60 Hz;
2) reacting the obtained dispersion solution for 24 hours under the heating condition, wherein the reaction temperature is 80-110 ℃, and the reaction is finished under the inert gas atmosphere (comprising nitrogen, argon and the like);
3) and removing impurities from the reacted mixed solution by a centrifugal separation method (the impurity removal process comprises: centrifugally collecting a solid product, ultrasonically dispersing the solid product in methylbenzene, centrifugally collecting the solid product again, and repeating the steps for three times) to prepare mSiO2-C8F13H4。
The preparation method provided by the invention is simple and feasible, has no corrosion, no environmental pollution, simple process and low cost, and can be suitable for large-scale industrial production.
Further, mSiO2-C8F13H4Drying for 48-72 hours at 55-65 ℃ under vacuum condition before preparing the composite material.
Vacuum is selected, the temperature is 55-65 ℃ for better removing the solvent, the nanoparticles are easy to agglomerate when the temperature is too high, and the solvent removing effect is limited when the temperature is too low.
Further, the prepared crosslinked polyethylene composite material is subjected to heat treatment in a vacuum oven at 82-85 ℃ for 48 hours to eliminate byproducts.
And (3) removing by-products at 82-85 ℃, and the applicant finds that: at the temperature, small molecules and unreacted substances generated in the preparation process of the composite material can be effectively removed.
The application of the crosslinked polyethylene composite material with the super-hydrophobic characteristic is to apply the crosslinked polyethylene composite material to a cable.
The crosslinked polyethylene composite material provided by the invention can be used as a main insulating material of a cable, effectively inhibits the defects of cable water tree degradation and the like caused by water vapor, moisture and other factors, and greatly improves the operation safety and stability of the cable.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the invention relates to mesoporous nano silicon dioxide (mSiO) with the surface modified with fluorine-containing functional molecules2-C8F13H4) The cable insulation material not only has porosity, but also has strong electronegativity of fluorine atoms, enhances the interface effect with crosslinked polyethylene by establishing intermolecular hydrogen bonds, reduces the surface free energy of the composite material, realizes the super-hydrophobic characteristic, and solves the problems that the existing crosslinked polyethylene cable insulation material is easy to be affected with damp and has poor hydrophobic effect.
2. The preparation method provided by the invention is simple and feasible, has no corrosion, no environmental pollution, simple process and low cost, and can be suitable for large-scale industrial production.
Drawings
The accompanying drawings, which are included to provide a further understanding of the embodiments of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention. In the drawings:
FIG. 1 is a schematic flow chart of mesoporous nano-silica surface modification of fluorine-containing functional molecules;
FIG. 2 is a contact angle of the composite materials obtained in examples 1 to 5 and comparative examples 1 to 2;
FIG. 3 is a graph showing the breakdown strength of the composite materials obtained in examples 1 to 5 and comparative examples 1 to 2;
FIG. 4 is a graph showing the volume resistivity of the composite materials obtained in examples 1 to 5 and comparative examples 1 to 2;
FIG. 5 is a comparison of the contact angles of the composites obtained in examples 1, 6, 7 and comparative examples 3, 4, 5.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples and accompanying drawings, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not meant to limit the present invention.
Example 1:
as shown in FIG. 1, a crosslinked polymer having superhydrophobic propertyThe ethylene composite material takes low-density polyethylene as a matrix, takes mesoporous nano-silica with fluorine-containing functional molecules modified on the surface as a filler, wherein the mass ratio of the matrix to the filler is 81:19, the mesoporous nano-silica is modified by triethoxy-1H, 1H,2H, 2H-tridecafluoro n-octylsilane, and the mass ratio of the triethoxy-1H, 1H,2H, 2H-tridecafluoro n-octylsilane to the mesoporous nano-silica is 0.2: 1; the density of the low-density polyethylene is 0.912g/m3Molecular weight is 146500; the average particle diameter of the mesoporous nano-silica is 50nm, and the average pore diameter is 0.6 nm.
The preparation method of the crosslinked polyethylene composite material with the super-hydrophobic characteristic comprises the following steps:
and 6, crosslinking the sample obtained in the step 5 at 170 ℃ and 15MPa for about 30min by adopting a flat vulcanizing machine, and carrying out heat treatment for 48 hours at 85 ℃ in a vacuum oven to obtain the composite material.
Example 2:
this example is based on example 1, and differs from example 1 in that: low density polyethylene and mSiO2-C8F13H4The mass ratio is 78: 22.
Example 3:
this example is based on example 1, and differs from example 1 in that: low density polyethylene and mSiO2-C8F13H4The mass ratio is 75: 25.
Example 4:
this example is based on example 1, and differs from example 1 in that: low density polyethylene and mSiO2-C8F13H4The mass ratio is 72: 28.
Example 5:
this example is based on example 1, and differs from example 1 in that: low density polyethylene and mSiO2-C8F13H4The mass ratio is 68: 32.
Example 6:
the cross-linked polyethylene composite material with the super-hydrophobic characteristic takes low-density polyethylene as a matrix and mesoporous nano-silica with fluorine-containing functional molecules modified on the surface as a filler, wherein the mass ratio of the matrix to the filler is 68:32, the mesoporous nano-silica is modified by triethoxy-1H, 1H,2H, 2H-tridecafluoro n-octylsilane, and the mass ratio of the triethoxy-1H, 1H,2H, 2H-tridecafluoro n-octylsilane to the mesoporous nano-silica is 0.4: 1; the density of the low-density polyethylene is 0.924g/m3Molecular weight is 179500; the average particle size of the mesoporous nano-silica is 100nm, and the average pore diameter is 5 nm.
The preparation method of the crosslinked polyethylene composite material with the super-hydrophobic characteristic comprises the following steps:
and 6, crosslinking the sample obtained in the step 5 for about 50min at 1704 ℃ and 13MPa by adopting a flat vulcanizing machine, and performing heat treatment for 48 hours at 82 ℃ in a vacuum oven to obtain the composite material.
Example 7:
this example is based on example 6, and differs from example 6 in that: the mass ratio of the triethoxy-1H, 1H,2H, 2H-tridecafluoro-n-octylsilane to the mesoporous nano-silica is 0.2: 1.
comparative example 1:
this comparative example is based on example 1 and differs from example 1 in that: low density polyethylene and mSiO2-C8F13H4The mass ratio is 95: 5.
Comparative example 2:
this comparative example is based on example 1 and differs from example 1 in that: the mass ratio of the low-density polyethylene to the mSiO2-C8F13H4 is 60: 40.
Comparative example 3:
this comparative example is based on example 1 and differs from example 1 in that: the mass ratio of the triethoxy-1H, 1H,2H, 2H-tridecafluoro-n-octylsilane to the mesoporous nano-silica is 0.05: 1.
Comparative example 4:
this comparative example is based on example 1 and differs from example 1 in that: the mass ratio of the triethoxy-1H, 1H,2H, 2H-tridecafluoro-n-octylsilane to the mesoporous nano-silica is 0.5: 1.
Comparative example 5:
this comparative example is based on example 1 and differs from example 1 in that: and (3) modifying the mesoporous nano silicon dioxide by using n-octyl triethoxysilane instead of triethoxy-1H, 1H,2H, 2H-tridecafluoro-n-octyl silane.
The composite materials prepared in the examples 1 to 7 and the comparative examples 1 to 5 are respectively subjected to performance tests: preparing the prepared composite material into a sample with a certain thickness according to the test requirement, and testing the contact angle, the breakdown strength and the direct-current resistivity; the method comprises the following specific steps: (1) the static contact angle of the sample surface was measured using a contact angle tester, the volume of the water drop was about 5. mu.L, and the average value of the contact angles at 5 different points on the sample surface was taken as the measurement result. (2) And (3) automatically boosting the pressure of the prepared composite material sample in silicone oil by adopting a ball-to-ball electrode, carrying out a breakdown experiment, and repeating each group of samples for 5 times. (3) The volume resistivity of the composite was measured using a high resistivity gecky meter 6517B. The results are shown in FIGS. 2 to 5 (wherein, in FIGS. 3 and 4, 1 to 5 on the abscissa correspond to examples 1 to 5, respectively), and it can be seen that the contact angles of the composites obtained in examples 1 to 5 are all greater than 150 ° while retaining excellent insulation properties (breakdown strength >35kV/mm, volume resistivity > 1015. omega. m). The contact angle of the composite material obtained in comparative example 1 is less than 150 degrees, and the requirement of the super-hydrophobic property is not met, mainly because the nano filler is too little to improve the hydrophobic property of the composite material. The contact angle of the composite material obtained in comparative example 2 was more than 150 deg., however, the breakdown strength was drastically decreased by about 34.3kV/mm, and it was found that the processing characteristics of the composite material in comparative example 2 were deteriorated. Thus, it can be concluded that either too high or too low a content of nanofiller affects the overall properties of the composite. The contact angle of the composite material of comparative example 3 is smaller than that of example 1, and the contact angle of comparative example 4 is close to that of example 1, indicating that when the ratio of the modifier to the mesoporous nano-silica is greater than 0.2:1, increasing the amount of the modifier does not greatly affect the contact angle of the composite material, and when the ratio of the amount of the modifier to the mesoporous nano-silica is 0.05:1, the contact angle of the composite material is reduced because the grafting amount of the functional molecule is insufficient. When the modifier was replaced with a non-fluorine-containing modifier of the same chain length, the contact angle of comparative example 5 was significantly smaller than example 1, fully demonstrating that the fluorine-containing functional molecule plays an important role in improving the hydrophobic properties of the composite.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (6)
1. The crosslinked polyethylene composite material with the super-hydrophobic characteristic is characterized in that low-density polyethylene is taken as a matrix, and mesoporous nano-silica with fluorine-containing functional molecules modified on the surface is taken as a filler; the mass percentages of the filler and the matrix are as follows: 19% -32.8%: 81% -67.2%; the modifier used for modifying the mesoporous nano-silica is triethoxy-1H, 1H,2H, 2H-tridecafluoro-n-octylsilane; the mass ratio of the modifier to the mesoporous nano silicon dioxide is as follows: 0.2-0.4: 1; the average particle size of the mesoporous nano-silica is 50-100 nm, and the average pore diameter is 0.6-5 nm;
the preparation method of the crosslinked polyethylene composite material comprises the following steps:
1) and prepolymer blending: mixing low-density polyethylene and mesoporous nano-silica, and then melting and blending at 105-110 ℃ to obtain a blending prepolymer compound with filler particles uniformly dispersed in crosslinked polyethylene;
2) blending the prepolymer and the crosslinking agent: melting and blending the blending prepolymer compound and dicumyl peroxide at 108-110 ℃ to obtain a ternary blending compound;
3) and hot-press forming: hot-pressing and molding the ternary blend compound under the conditions of 13-15 Mpa and 108-115 ℃ by adopting a flat vulcanizing machine to prepare a sample;
4) and vulcanization crosslinking: and crosslinking the sample for 30-50min at 168-174 ℃ and 13-16MPa by adopting a flat vulcanizing machine to obtain the crosslinked polyethylene composite material.
2. The crosslinked polyethylene composite material with superhydrophobic property according to claim 1, wherein the low density polyethylene has a density of 0.912-0.924 g/cm and molecular weight of 146500-179500 when subjected to thin film cultivation.
3. A method for preparing a crosslinked polyethylene composite material having superhydrophobic properties according to any one of claims 1-2, comprising the steps of:
1) and prepolymer blending: mixing low-density polyethylene and mesoporous nano-silica, and then melting and blending at 105-110 ℃ to obtain a blending prepolymer compound with filler particles uniformly dispersed in crosslinked polyethylene;
2) blending the prepolymer and the crosslinking agent: melting and blending the blending prepolymer compound and dicumyl peroxide at 108-110 ℃ to obtain a ternary blending compound;
3) and hot-press forming: hot-pressing and molding the ternary blend compound under the conditions of 13-15 Mpa and 108-115 ℃ by adopting a flat vulcanizing machine to prepare a sample;
4) and vulcanization crosslinking: and crosslinking the sample for 30-50min at 168-174 ℃ and 13-16MPa by adopting a flat vulcanizing machine to obtain the crosslinked polyethylene composite material.
4. The method for preparing the crosslinked polyethylene composite material with the superhydrophobic property of claim 3, wherein the mesoporous nano silica is dried at 55-65 ℃ for 48-72 hours under vacuum condition before preparing the composite material.
5. The method for preparing a crosslinked polyethylene composite material with superhydrophobic property according to claim 3, wherein the prepared crosslinked polyethylene composite material is heat-treated at 82-85 ℃ for 48 hours in a vacuum oven to eliminate by-products.
6. Use of a crosslinked polyethylene composite with superhydrophobic properties according to any of claims 1-2, wherein said crosslinked polyethylene composite is used in cables.
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| "温度对聚乙烯水树枝老化特性的影响";王金锋 等;《高电压技术》;20120131;第38卷(第1期);第1.2节 * |
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| CN110452444A (en) | 2019-11-15 |
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