CN114806117B - Polylactic acid shell of electric energy metering box and preparation method thereof - Google Patents
Polylactic acid shell of electric energy metering box and preparation method thereof Download PDFInfo
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- CN114806117B CN114806117B CN202210535045.3A CN202210535045A CN114806117B CN 114806117 B CN114806117 B CN 114806117B CN 202210535045 A CN202210535045 A CN 202210535045A CN 114806117 B CN114806117 B CN 114806117B
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K5/05—Alcohols; Metal alcoholates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2275—Ferroso-ferric oxide (Fe3O4)
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention discloses a polylactic acid shell of an electric energy metering box and a preparation method thereof. The preparation method of the invention comprises the following steps: placing the phase change material, the high molecular surfactant and the alcohol-water mixed solution into a reaction container for mixing; under the protection of inert gas, a temperature control system is started to heat the reaction system to 30-100 ℃; after the temperature of the reaction system is stable, adding the styrene monomer and the initiator, mixing and stirring, wherein the stirring speed is 200-400r/min; when reacting for 11-13h, adding the ferromagnetic nano particles modified by the high molecular surfactant, and continuing to react for 2-4h to obtain the phase-change microcapsule; placing polylactic acid into a dryer, and drying at 55-65deg.C for 22-26 hr to remove water; premixing polylactic acid and phase-change microcapsules, and carrying out melt extrusion and granulation by a double-screw extruder; and carrying out injection molding on the blended particles by an injection molding machine. The invention can effectively inhibit the development of electric branches, delay the electric aging process of materials, prolong the service life of the materials and improve the use safety.
Description
Technical Field
The invention belongs to the technical field of electrical materials, and particularly relates to a polylactic acid shell of an electric energy metering box and a preparation method thereof.
Background
Polylactic acid is a novel green polymer material, has the characteristics of excellent biocompatibility, biodegradability, high strength and the like, has good electrical property and mechanical property, is popularized and applied in the fields of low-voltage energy metering box shells, power electronic devices and the like at present, and particularly can cause the electric energy metering box polylactic acid shells to generate local defects such as bubbles, microcracks and the like under the complex working condition conditions such as rain, strong light irradiation, high temperature and the like, and can induce electrical aging processes such as electrical branches and the like under the action of an electric field, so that the shell material is damaged in insulation and the electrical and mechanical properties are invalid due to further development.
Therefore, if the development of the electric branch can be restrained, the development process of the electric aging can be delayed, and the service life of the polylactic acid shell of the electric energy metering box can be effectively prolonged.
Disclosure of Invention
Based on the problem that discharge defects such as electric branches appear in the interior of the polylactic acid shell of the existing electric energy metering box, the invention provides the polylactic acid shell of the electric energy metering box doped with the phase change microcapsule capable of inhibiting partial discharge of the polylactic acid and the preparation method thereof, so that the safety performance and long-term stability of the polylactic acid shell of the electric energy metering box serving as electric equipment are improved.
Therefore, the invention adopts the following technical scheme: the preparation method of the polylactic acid shell of the electric energy metering box comprises the following steps:
step 3, adding a mixture of a styrene monomer and an initiator and stirring after the system temperature is stable, wherein the stirring speed is 200-400r/min;
step 4, adding the ferromagnetic nano particles modified by the high molecular surfactant when reacting for 11-13 hours, and continuing to react for 2-4 hours to obtain MA@PS@Fe 3 O 4 Phase change microcapsules;
step 5, placing the polylactic acid into a dryer, and drying at 55-65 ℃ for 22-26 hours to remove water;
step 6, polylactic acid and MA@PS@Fe 3 O 4 Premixing phase-change microcapsules, and carrying out melt extrusion and granulation by a double-screw extruder;
and 7, carrying out injection molding on the blended particles by an injection molding machine.
Aiming at the characteristics of formation and development of electric branches of the polylactic acid shell material of the electric energy metering box, the phase-change microcapsule and the polylactic acid are blended to prepare the polylactic acid material containing the phase-change microcapsule, in the process of electric aging, ferromagnetic nano particles on the surface of the phase-change microcapsule have a guiding effect on the development of the electric branches, and when the electric branches develop to the vicinity of the phase-change microcapsule, heat released by the development process of the electric branches causes the phase-change material to absorb heat and change phase, so that the development of the electric branches is inhibited, and the development process of the electric aging is further delayed, thereby achieving the purpose of realizing the electric aging resistance of the polylactic acid shell material of the electric energy metering box by utilizing the phase-change microcapsule.
Preferably, in step 1, the mixed materials are stirred in the reaction vessel at a speed of 100-200 r/min.
Preferably, in step 4, the material after 2-4 hours of reaction is centrifugally dried.
Preferably, in the step 6, the mass fraction ratio of the polylactic acid to the MA@PS@Fe3O4 phase change microcapsule is 99.9:0.1, controlling the extrusion temperature from a feed inlet to a die head at 100-180 ℃ and the rotating speed of a screw rod at 200-300r/min to obtain the polylactic acid shell material particles of the phase change microcapsule which are doped and can realize electric aging resistance.
Preferably, in the step 7, the extrusion temperature from a feed inlet to a die head is controlled to be 150-210 ℃, so that the polylactic acid shell of the phase change microcapsule which is doped and can realize electrical aging resistance is obtained.
Preferably, the dosage ratio of the phase change material, the macromolecular surfactant and the alcohol-water mixed solution is 3-5ml:1g:15-25ml; the alcohol-water mixed solution consists of ethanol and water, wherein the volume ratio of the ethanol to the water is 90-99:1-10.
Preferably, the phase change material is tetradecanol.
Preferably, the polymer surfactant is sodium dodecyl benzene sulfonate.
Preferably, the initiator is Azobisisobutyronitrile (AIBN).
The polylactic acid shell material of the electric energy metering box has the following characteristics:
(1) The phase change microcapsule in the polylactic acid shell material of the electric energy metering box is of a monodisperse core-shell structure.
(2) The surface of the phase change microcapsule in the polylactic acid shell material of the electric energy metering box contains ferromagnetic nano particles, and has a guiding effect on the development of electric branches.
(3) The phase change microcapsule in the polylactic acid shell material of the electric energy metering box has the capacity of absorbing heat and phase change, and has better energy storage and temperature adjustment effects in the polylactic acid shell material of the electric energy metering box.
(4) The phase change microcapsule of the polylactic acid shell material of the electric energy metering box can effectively inhibit the development of the electric branches in the polylactic acid shell material of the electric energy metering box by combining the heat absorption and transformation capacity of the internal phase change material through the induction effect of the surface ferromagnetic nano particles on the development of the electric branches, delay the electric aging process of the material, prolong the service life of the material and improve the use safety.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) image of a phase change microcapsule without added ferromagnetic nanoparticles in the present invention;
FIG. 2 is an energy spectrum (EDS) diagram of a phase change microcapsule incorporating ferromagnetic nanoparticles according to the present invention;
FIG. 3 is a diagram showing the shape of an electrical branch when the pressure of the polylactic acid shell material of the low-voltage electric energy metering box is 60 minutes without adding phase change microcapsules;
FIG. 4 is a diagram showing the shape of an electrical branch when the polylactic acid shell material of the electrical energy metering box added with the phase change microcapsule is subjected to pressure resistance for 60 minutes;
FIG. 5 is a graph of partial discharge signals when the polylactic acid shell material of the low-voltage electric energy metering box is pressure-resistant for 60min without adding phase-change microcapsules;
FIG. 6 is a graph showing partial discharge signals when the polylactic acid casing material of the electric energy metering box to which the phase change microcapsule is added is subjected to pressure resistance for 60 minutes.
Detailed Description
The invention is described in detail below with reference to the drawings and the detailed description.
Microcapsules are special core materials, and after microencapsulation treatment, the color, morphological properties and the like of the core materials are changed to a certain extent, and under specific conditions, the core materials are activated to play a role. According to the invention, the phase change microcapsule with the ferromagnetic nano particles is added, the ferromagnetic nano particles are utilized to induce the development of the electric branch to the microcapsule, and meanwhile, the principle that the development speed of the electric branch can be effectively realized by absorbing heat of the phase change material is utilized, so that the purpose of resisting the electric aging of the polylactic acid shell material of the electric energy metering box is realized.
The specific preparation method of the polylactic acid shell of the electric energy metering box comprises the following steps:
step 1: the phase change material tetradecanol, the high molecular surfactant and the alcohol-water mixed solution are placed in a flask to be mixed.
Step 2: under the protection of inert gas, a temperature control system is started to heat the reaction system to 30-100 ℃.
Step 3: after the temperature of the reaction system is stable, adding the styrene monomer and the initiator Azodiisobutyronitrile (AIBN), mixing and stirring, wherein the stirring speed is 200-400r/min.
Step 4: when the reaction is carried out for 12 hours, adding the ferromagnetism nanometer particles modified by sodium dodecyl benzene sulfonate, and continuing the reaction for 2-4 hours.
Step 5: placing polylactic acid into a dryer, and drying at 55-65deg.C for 22-26 hr to remove water.
Step 6: polylactic acid and MA@PS@Fe3O4 phase change microcapsules are mixed according to the mass fraction ratio of 99.9:0.1 premixing, and carrying out melt extrusion and granulation by a double-screw extruder.
Step 7: and carrying out injection molding on the blended particles by an injection molding machine.
Specifically, in step 1, the mixed materials are stirred in a beaker at a speed of 100-200 r/min.
Specifically, in the step 4, the material after 2-4 hours of reaction is centrifugally dried.
Specifically, in the step 6, the extrusion temperature from a feed inlet to a die head is controlled at 100-180 ℃, the rotating speed of a screw is 200-300r/min, and the polylactic acid shell material particles of the phase change microcapsule which can realize electrical aging resistance and are doped are obtained.
Specifically, in the step 7, the extrusion temperature from a feed inlet to a die head is controlled to be 150-210 ℃, so that the polylactic acid shell of the electric energy metering box doped with the phase change microcapsule capable of realizing electric aging resistance is obtained.
Specifically, the macromolecular surfactant is sodium dodecyl benzene sulfonate.
Specifically, the dosage ratio of the phase change material, the macromolecular surfactant and the alcohol-water mixed solution is 3-5ml:1g:15-25ml, most preferably 5ml:1g:20ml; the alcohol-water mixed solution consists of ethanol and water, wherein the volume ratio of the ethanol to the water is 90-99:1-10, most preferably 95:5.
the embodiment of the invention prepares the polylactic acid shell of the electric energy metering box doped with the phase change microcapsule capable of realizing electric aging resistance.
Fig. 1 shows that the phase-change microcapsule of the undoped ferromagnetic nanoparticle is subjected to Scanning Electron Microscope (SEM) analysis, and the phase-change microcapsule has a monodisperse spherical structure, a particle size of about 9 μm and a uniform size.
Fig. 2 shows that the phase change microcapsule doped with the ferromagnetic nanoparticles is subjected to energy spectrum (EDS) analysis, and a large amount of iron elements are uniformly distributed on the surface of the phase change microcapsule modified by the ferromagnetic nanoparticles, so that the ferromagnetic nanoparticles are combined with the microsphere surface. The ferromagnetic nano particles modify the surface of the microsphere, and have the function of guiding the electric branch to develop to the vicinity of the phase-change microcapsule.
Fig. 3 to 4 are electrical branch shapes of the polylactic acid casing material of the low-voltage electrical energy metering box without adding the phase-change microcapsule and the polylactic acid casing material of the electrical energy metering box with adding the phase-change microcapsule, which withstand voltage for 60 min. Partial discharge of the material in the insulating layer due to excessive concentrated field strength causes dendritic ageing of the insulating material, known as electrical dendrites. As can be seen from the graph, when the withstand voltage time is 60min, the longitudinal lengths of the electric branches in the polylactic acid shell material of the low-voltage electric energy metering box without adding the phase-change microcapsules and the polylactic acid shell material of the electric energy metering box with adding the phase-change microcapsules are 342.4 mu m and 312.5 mu m respectively, and the transverse lengths are 541.8 mu m and 296.7 mu m respectively. The electric branches in the polylactic acid shell material of the electric energy metering box containing the phase-change microcapsules are in a dense cluster shape, the electric branches in the polylactic acid shell material of the electric energy metering box without the phase-change microcapsules are sparse, and the longitudinal and transverse lengths are respectively reduced by 8.7 percent and 45.2 percent. The phase change microcapsule effectively inhibits the growth of electric branches in the polylactic acid shell material of the low-voltage electric energy metering box, and improves the dielectric property of the polylactic acid shell material of the low-voltage electric energy metering box.
Fig. 5 to 6 are partial discharge signal diagrams of the polylactic acid shell material of the low-voltage electric energy metering box without adding the phase change microcapsule and the polylactic acid shell material of the electric energy metering box with adding the phase change microcapsule for 60 minutes, respectively, and it can be seen from the diagrams that the partial discharge inside the sample mainly occurs in the stage of gradually increasing the power frequency alternating voltage, and the influence of the withstand voltage time is small. When the voltage is 60min, the average discharge amplitude of the polylactic acid shell material of the electric energy metering box without the phase change microcapsule is 1.73mV, the average discharge amplitude of the polylactic acid shell material of the electric energy metering box with the phase change microcapsule is 1.12mV, the average discharge amplitude is reduced by 35.2%, the partial discharge intensity in the polylactic acid shell material of the electric energy metering box is weakened, the partial discharge process is restrained, and the phase change microcapsule has an inhibiting effect on the development of electric branches in the polylactic acid shell material of the electric energy metering box, so that the electric aging resistance effect of the polylactic acid shell material of the electric energy metering box can be realized.
Claims (7)
1. The preparation method of the polylactic acid shell of the electric energy metering box is characterized by comprising the following steps:
step 1, placing a phase change material, a high molecular surfactant and an alcohol-water mixed solution in a reaction container for mixing;
step 2, under the protection of inert gas, starting a temperature control system to heat the reaction system to 30-100 ℃;
step 3, adding a styrene monomer and an initiator to mix and stir after the temperature of the reaction system is stable, wherein the stirring speed is 200-400r/min;
step 4, adding the ferromagnetic nano particles modified by the high molecular surfactant when reacting for 11-13 hours, and continuing to react for 2-4 hours to obtain MA@PS@Fe 3 O 4 Phase change microcapsules;
step 5, placing the polylactic acid into a dryer, and drying at 55-65 ℃ for 22-26 hours to remove water;
step 6, polylactic acid and MA@PS@Fe 3 O 4 Premixing phase-change microcapsules, and carrying out melt extrusion and granulation by a double-screw extruder;
step 7, injection molding the blended particles by an injection molding machine;
the dosage ratio of the phase change material, the macromolecular surfactant and the alcohol-water mixed solution is 3-5ml:1g:15-25ml; the alcohol-water mixed solution consists of ethanol and water, wherein the volume ratio of the ethanol to the water is 90-99:1-10;
the phase change material is tetradecyl alcohol;
the macromolecular surfactant is sodium dodecyl benzene sulfonate.
2. The method for producing an electric-energy metering box polylactic acid casing according to claim 1, wherein in step 1, the mixed materials are stirred in a reaction vessel at a speed of 100 to 200 r/min.
3. The method for preparing the polylactic acid shell of the electric energy metering box according to claim 1, wherein in the step 4, the material after 2-4 hours of reaction is centrifugally dried.
4. The method for preparing the polylactic acid shell of the electric energy metering box according to claim 1, wherein in the step 6, the mass fraction ratio of polylactic acid to MA@PS@Fe3O4 phase change microcapsules is 99.9:0.1, controlling the extrusion temperature from a feed inlet to a die head at 100-180 ℃ and the rotating speed of a screw rod at 200-300r/min to obtain the polylactic acid shell material particles of the phase change microcapsule which are doped and can realize electric aging resistance.
5. The method for preparing the polylactic acid shell of the electric energy metering box according to claim 1, wherein in the step 7, the extrusion temperature from a feed inlet to a die head is controlled to be 150-210 ℃, so that the polylactic acid shell of the phase change microcapsule which is doped and can realize electric aging resistance is obtained.
6. The method for preparing the polylactic acid shell of the electric energy metering box according to claim 1, wherein the initiator is azobisisobutyronitrile.
7. An electric energy metering box polylactic acid casing prepared by the preparation method of any one of claims 1 to 6.
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| US20170107413A1 (en) * | 2015-10-19 | 2017-04-20 | Liang Wang | Anti-icing composition driven by catalytic hydrogen generation under subzero temperatures |
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| CN106633317A (en) * | 2017-01-10 | 2017-05-10 | 重庆大学 | Preparation method for cable insulating material capable of realizing self-repairing of early-stage electrical-tree defects |
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