CN114806117A - 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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- CN114806117A CN114806117A CN202210535045.3A CN202210535045A CN114806117A CN 114806117 A CN114806117 A CN 114806117A CN 202210535045 A CN202210535045 A CN 202210535045A CN 114806117 A CN114806117 A CN 114806117A
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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
- 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
- C08K3/22—Oxides; Hydroxides of metals
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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
- C08K5/00—Use of organic 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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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
- 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
- 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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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: putting the phase change material, the high molecular surfactant and the alcohol-water mixed solution into a reaction container for mixing; starting a temperature control system to heat the reaction system to 30-100 ℃ under the inert gas protection atmosphere; when the temperature of the reaction system is stable, adding a styrene monomer and an initiator, mixing and stirring at the stirring speed of 200-400 r/min; when the reaction lasts for 11-13h, adding ferromagnetic nanoparticles modified by a high molecular surfactant, and continuing the reaction for 2-4h to obtain phase-change microcapsules; putting the polylactic acid into a dryer, drying for 22-26h at 55-65 ℃, and removing water; premixing polylactic acid and phase change microcapsules, and performing melt extrusion and granulation by a double-screw extruder; and (3) injection molding the blended particles by an injection molding machine. The invention can effectively inhibit the development of the electric tree, delay the electric aging process of the material, prolong the service life of the material 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 characteristics such as excellent biocompatibility, biodegradability and high strength, has good electrical properties and mechanical properties simultaneously, has been popularized and applied in fields such as low voltage electric energy metering box shell, power electronics at present, especially electric energy metering box polylactic acid shell, under complicated operating mode condition, such as rain, strong light irradiation, high temperature, can lead to electric energy metering box polylactic acid shell to produce local defects such as bubble, crazing line, etc., induce electric branch isoaging process under the effect of electric field, further development will lead to shell material insulation damage, cause electrical and mechanical properties to become invalid.
Therefore, if the development of the electric tree can be inhibited and the development process of the electric aging is delayed, 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 tree branches and the like occur in the polylactic acid shell of the conventional electric energy metering box, the invention provides the polylactic acid shell of the electric energy metering box doped with the phase-change microcapsules capable of inhibiting partial discharge of polylactic acid and the preparation method thereof, so that the safety performance and the long-term stability of the polylactic acid shell of the electric energy metering box as power equipment are improved.
Therefore, the invention adopts the following technical scheme: a preparation method of a polylactic acid shell of an electric energy metering box comprises the following steps:
step 3, after the temperature of the system is stable, adding a styrene monomer and an initiator mixture and stirring at a stirring speed of 200-400 r/min;
step 4, when the reaction lasts for 11-13h, adding the ferromagnetic nanoparticles modified by the macromolecular surfactant, and continuing the reaction for 2-4h to obtain MA @ PS @ Fe 3 O 4 Phase change microcapsules;
step 5, putting the polylactic acid into a dryer, drying for 22-26h at 55-65 ℃, and removing water;
step 6, mixing polylactic acid and MA @ PS @ Fe 3 O 4 Pre-mixing the phase-change microcapsules, and performing melt extrusion and granulation by a double-screw extruder;
and 7, injection molding the blended particles by an injection molding machine.
Aiming at the characteristics of formation and development of polylactic acid shell materials of electric energy metering boxes, the phase-change microcapsules and polylactic acid are blended to prepare the polylactic acid materials containing the phase-change microcapsules, ferromagnetic nanoparticles on the surfaces of the phase-change microcapsules have a guiding effect on development of the electric branches in an electric aging process, and when the electric branches develop to the vicinity of the phase-change microcapsules, heat released in the development process of the electric branches causes heat absorption phase change of the phase-change materials, so that the development of the electric branches is inhibited, and further, the development process of the electric aging is delayed, and therefore, the aim of utilizing the phase-change microcapsules to achieve the anti-electric aging of the polylactic acid shell materials of the electric energy metering boxes is fulfilled.
Preferably, in step 1, the mixed material is stirred in the reaction vessel at a speed of 100-.
Preferably, in step 4, the material after 2-4h of reaction is dried by centrifugation.
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 the feed inlet to the die head at 180 ℃ and controlling the screw rotation speed at 300r/min and 200-.
Preferably, in the step 7, the extrusion temperature from the feed inlet to the die head is controlled at 150-210 ℃, and the low-voltage electric energy metering box polylactic acid shell doped with the anti-electrical-aging phase-change microcapsules is obtained.
Preferably, the dosage ratio of the phase-change material, the high-molecular surfactant and the alcohol-water mixed solution is 3-5 ml: 1 g: 15-25 ml; the alcohol-water mixed solution consists of ethanol and water, and the volume ratio of the ethanol to the water is 90-99: 1-10.
Preferably, the phase change material is tetradecanol.
Preferably, the polymeric 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 the phase change microcapsule has a guiding effect on development of electric branches.
(3) The phase change microcapsules in the polylactic acid shell material of the electric energy metering box have the capacity of absorbing heat and changing phase, and show a good energy storage and temperature regulation effect 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 tree in the polylactic acid shell material of the electric energy metering box by combining the heat absorption phase change capability of the internal phase change material through the induction effect of the surface ferromagnetic nano particles on the development of the electric tree, 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;
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 of the shape of the electric tree of the low-voltage electric energy metering box polylactic acid shell material without phase change microcapsules when the material is subjected to pressure resistance for 60 min;
FIG. 4 is a diagram of the shape of an electric tree of the electric energy metering box polylactic acid shell material with the phase-change microcapsule added therein, which resists pressure for 60 min;
FIG. 5 is a partial discharge signal diagram of the low-voltage electric energy metering box polylactic acid casing material without phase change microcapsule for 60 min;
FIG. 6 is a partial discharge signal diagram of the electric energy metering box polylactic acid shell material with the phase change microcapsule added to withstand the pressure for 60 min.
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, the color, morphological properties, etc. of the microcapsules are changed to some extent, and under specific conditions, the core materials are activated to function. According to the invention, the phase change microcapsule added with the ferromagnetic nanoparticles is utilized, and the aim of resisting electrical aging of the polylactic acid shell material of the electric energy metering box is fulfilled by utilizing the principle that the ferromagnetic nanoparticles induce the development of electrical tree branches into the microcapsule and the phase change material absorbs heat to effectively accelerate the development speed of the electrical tree branches.
The specific preparation method of the polylactic acid shell of the electric energy metering box comprises the following steps:
step 1: placing the phase change material tetradecanol, the high molecular surfactant and the alcohol-water mixed solution into a flask for mixing.
Step 2: under the condition of inert gas protective atmosphere, starting a temperature control system to heat the reaction system to 30-100 ℃.
And 3, step 3: when the temperature of the reaction system is stable, adding a styrene monomer and an initiator Azobisisobutyronitrile (AIBN), mixing and stirring at the stirring speed of 200-400 r/min.
And 4, step 4: when the reaction is carried out for 12 hours, the ferromagnetic nano-particles modified by the sodium dodecyl benzene sulfonate are added, and the reaction is continued for 2 to 4 hours.
And 5: putting the polylactic acid into a dryer, drying for 22-26h at 55-65 ℃, and removing water.
Step 6: the phase-change microcapsule of polylactic acid and MA @ PS @ Fe3O4 is prepared according to the mass fraction ratio of 99.9: 0.1 pre-mixing, melting and extruding by a double-screw extruder, and granulating.
And 7: and (3) injection molding the blended particles by an injection molding machine.
Specifically, in step 1, the mixed material was stirred in a beaker at a speed of 100-.
Specifically, in step 4, the material after 2-4h of reaction is centrifugally dried.
Specifically, in the step 6, the extrusion temperature from the feed inlet to the die head is controlled at 180 ℃ and the screw rotation speed is controlled at 300r/min, so as to obtain the polylactic acid shell material particles of the low-voltage electric energy metering box doped with the phase-change microcapsules capable of realizing the electrical aging resistance.
Specifically, in step 7, the extrusion temperature from the feed inlet to the die head is controlled at 150-.
Specifically, the macromolecular surfactant is sodium dodecyl benzene sulfonate.
Specifically, the dosage ratio of the phase-change material, the high molecular surfactant and the alcohol-water mixed solution is 3-5 ml: 1 g: 15-25ml, most preferably 5 ml: 1 g: 20ml of the solution; the alcohol-water mixed solution consists of ethanol and water, and 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 the anti-electrical ageing.
Fig. 1 shows Scanning Electron Microscope (SEM) analysis of phase-change microcapsules without doped ferromagnetic nanoparticles, wherein the phase-change microcapsules have a monodisperse spherical structure, a particle size of about 9 μm, and a uniform size.
Fig. 2 is an energy spectrum (EDS) analysis of the phase change microcapsule doped with ferromagnetic nanoparticles, and the surface of the phase change microcapsule modified with ferromagnetic nanoparticles has a uniform distribution of a large amount of iron elements, indicating that the ferromagnetic nanoparticles are bonded to the surface of the microsphere. The ferromagnetic nano particles modify the surface of the microsphere and have the function of guiding the development of the electric tree to the vicinity of the phase change microcapsule.
FIGS. 3 to 4 are diagrams of the shapes of the polylactic acid shell material of the low-voltage electric energy metering box without the phase-change microcapsule and the polylactic acid shell material of the electric energy metering box with the phase-change microcapsule for 60 min. Partial discharges of the material in the insulating layer due to excessively high concentrated field strengths lead to dendritic ageing of the insulating material, known as electrical dendrites. As can be seen from the figure, when the withstand voltage time is 60min, the longitudinal lengths of the electric tree branches in the polylactic acid shell material of the low-voltage power metering box without the phase-change microcapsule and the polylactic acid shell material of the power metering box with the phase-change microcapsule are 342.4 μm and 312.5 μm respectively, and the transverse lengths are 541.8 μm and 296.7 μm respectively. The electric tree in the polylactic acid shell material of the electric energy metering box containing the phase-change microcapsules is in a dense cluster shape, the electric tree in the polylactic acid shell material of the low-voltage electric energy metering box without the phase-change microcapsules is sparse, and the longitudinal length and the transverse length are respectively reduced by 8.7 percent and 45.2 percent. The phase change microcapsule effectively inhibits the growth of electric tree 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. 5-6 are partial discharge signal diagrams of the polylactic acid shell material of the low-voltage electric energy metering box without the phase-change microcapsule and the polylactic acid shell material of the electric energy metering box with the phase-change microcapsule for 60min of withstand voltage respectively, and it can be seen from the diagrams that the partial discharge inside the sample mainly occurs at the stage of gradually increasing power frequency alternating voltage and is less influenced by withstand voltage time. The discharge voltage amplitude is observed to find that when the voltage is withstand for 60min, the average discharge amplitude of the polylactic acid shell material of the low-voltage 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, and the average discharge amplitude is reduced by 35.2%, which shows that the internal partial discharge strength of the polylactic acid shell material of the electric energy metering box is weakened, and the partial discharge process is inhibited, thereby proving that the phase-change microcapsule has an inhibiting effect on the development of electrical branches in the polylactic acid shell material of the low-voltage electric energy metering box, and realizing the anti-electrical aging effect of the polylactic acid shell material of the electric energy metering box.
Claims (10)
1. A preparation method of a polylactic acid shell of an 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 into a reaction container for mixing;
step 2, starting a temperature control system to heat the reaction system to 30-100 ℃ under the inert gas protection atmosphere;
step 3, after the temperature of the reaction system is stable, adding a styrene monomer and an initiator, mixing and stirring at the stirring speed of 200-400 r/min;
step 4, when the reaction lasts for 11-13h, adding the ferromagnetic nano-particles modified by the macromolecular surfactant, and continuing the reaction for 2-4h to obtain MA @ PS @ Fe 3 O 4 Phase change microcapsules;
step 5, putting the polylactic acid into a dryer, drying for 22-26h at 55-65 ℃, and removing water;
step 6, mixing polylactic acid and MA @ PS @ Fe 3 O 4 Pre-mixing the phase-change microcapsules, and performing melt extrusion and granulation by a double-screw extruder;
and 7, injection molding the blended particles by an injection molding machine.
2. The method as claimed in claim 1, wherein in step 1, the mixed material is stirred in the reaction vessel at a speed of 100-200 r/min.
3. The preparation method of the polylactic acid casing 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 preparation method of 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 the feed inlet to the die head at 180 ℃ and controlling the screw rotation speed at 300r/min and 200-.
5. The preparation method of the polylactic acid casing of the electric energy metering box as claimed in claim 1, wherein in the step 7, the extrusion temperature from the feed inlet to the die head is controlled at 150 ℃ and 210 ℃ to obtain the low-voltage electric energy metering box polylactic acid casing doped with the anti-electrical aging phase-change microcapsules.
6. The preparation method of the polylactic acid shell of the electric energy metering box according to claim 1, wherein the dosage ratio of the phase-change material, the polymeric surfactant and the alcohol-water mixed solution is 3-5 ml: 1 g: 15-25 ml; the alcohol-water mixed solution consists of ethanol and water, and the volume ratio of the ethanol to the water is 90-99: 1-10.
7. The method for preparing the polylactic acid shell of the electric energy metering box according to claim 1, wherein the phase change material is tetradecanol.
8. The preparation method of the polylactic acid shell of the electric energy metering box according to claim 1, wherein the high molecular surfactant is sodium dodecyl benzene sulfonate.
9. The method for preparing the polylactic acid shell of the electric energy metering box according to claim 1, wherein the initiator is azobisisobutyronitrile.
10. An electric energy metering box polylactic acid shell prepared by the preparation method of any one of claims 1 to 9.
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