A high-adhesion PPS composite material, its preparation method and its application in capacitor casings
By combining modified PPS resin with toughening agents and other materials, and using PECVD plasma enhanced chemical vapor deposition method for graft copolymerization, the problem of decreased floor area ratio of PPS materials under high temperature and high humidity conditions and easy fall off with epoxy glue is solved, and the preparation of high adhesion PPS composite materials is realized, which significantly improves the sealing property and capacitance retention rate of the capacitor.
Patent Information
- Application Number
- CN202211733549.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2022-12-30
- Publication Date
- 2025-05-30
- Estimated Expiration
- 2042-12-30
AI Technical Summary
The existing PPS materials tend to cause the capacitor floor area ratio to decrease under high temperature and high humidity conditions, and the epoxy glue is easily fallen off, resulting in poor sealing.
Modified PPS resin is used as the main material, toughening agent, glass fiber, filler, coupling agent, chain extender, antioxidant and other additives are added, and graft copolymerization is carried out through PECVD plasma enhanced chemical vapor deposition method to improve adhesion and mechanical properties.
The weather resistance, heat resistance, mechanical strength and adhesion of PPS composite materials are significantly improved, ensuring that the sealing and capacitance retention of the capacitor are still good under high temperature and high humidity conditions.
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Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of PPS composite materials for capacitor housings, and specifically relates to a PPS composite material with high adhesion, a preparation method thereof, and an application thereof in capacitor housings. Background Art
[0002] In electronic and electrical components, capacitors play a very important role. They are essential basic components in electronic circuits and are collectively referred to as the three major passive components together with resistors and inductors.
[0003] In order to ensure the safety of capacitors during operation, it is often necessary to take potting protection measures for capacitors. Using epoxy resin ab potting adhesive as the filling material for capacitors can ensure excellent stability of the windings in the sealed housing, and at the same time has excellent insulation, flame retardant and other functions. Polyphenylene sulfide (PPS) as the base material of the capacitor housing needs to have good bonding performance with epoxy resin, and after being subjected to thermal cycling shock, the bonding interface will not crack. It also needs to meet the characteristics of high heat resistance, high mechanical strength, dimensional stability, high insulation, and anti-electric leakage. However, ordinary PPS materials generally have poor toughness, and the epoxy potting adhesive is prone to falling off, resulting in poor airtightness of the material. It is easy to reduce the capacitance rate of capacitors under high temperature and high humidity conditions and is difficult to meet the requirements. Summary of the Invention
[0004] In order to overcome the disadvantages and deficiencies existing in the prior art, one of the purposes of the present invention is to provide a PPS composite material with high adhesion, which has good bonding force with epoxy potting adhesive and is not easy to fall off, and can still maintain a good capacitance retention rate under high temperature and high humidity conditions.
[0005] Another purpose of the present invention is to provide a preparation method of a PPS composite material with high adhesion. The preparation method is simple to operate, convenient to control, has high production efficiency and low production cost, and can be used for large-scale production.
[0006] Another purpose of the present invention is to provide an application of a PPS composite material with high adhesion in capacitor housings. The PPS composite material with high adhesion is used as the base material for producing capacitor housings, and has excellent comprehensive performance, and at the same time has good high temperature and high humidity resistance characteristics. After testing for 1000 hours under the conditions of 85% humidity and 85°C, the surface epoxy bonding force is still very strong.
[0007] One of the purposes of the present invention is achieved by the following technical solution: A PPS composite material with high adhesion, comprising the following raw materials in parts by weight:
[0008]
[0009] The high-adhesion PPS composite material of the present invention uses modified PPS resin as the main material, and adds a toughening agent, glass fiber, filler, coupling agent, chain extender, antioxidant and other auxiliaries to further blend and modify the modified PPS resin. Through their synergistic effects, the toughness is improved, chain breakage is reduced, more excellent mechanical properties are obtained, more active groups are provided, the adhesion to epoxy resin is enhanced, the problem of easy peeling off when bonded to epoxy resin is avoided, and it is beneficial to maintain a high tightness with epoxy resin.
[0010] Preferably, the toughening agent is at least one of POE-g-GMA, ethylene-butyl acrylate copolymer EBA, ethylene-methyl acrylate copolymer EMA or SEBS-g-MAH.
[0011] Adopting the above technical solution is beneficial to increasing the toughness of the material, improving the weather resistance, heat resistance, compression set resistance and mechanical strength of the PPS composite material. At the same time, the active groups of the toughening agent enhance the epoxy binding force of the PPS composite material.
[0012] Preferably, the glass fiber is high-modulus chopped glass fiber.
[0013] Adopting the above technical solution has a lower warpage degree and better dimensional stability, helps to increase the fiber content and mechanical properties, enables the PPS composite material to have a higher impact strength, and can also reduce the warpage degree of the PPS composite material. Further, the elastic modulus of the high-modulus chopped glass fiber is 93.0 - 95.0 GPa, and the chopped length is 2.0 - 4.5 mm. After processing, the retained length of the glass fiber tends to the critical optimum length, further enhancing the mechanical properties such as the flexural modulus, tensile strength, compressive strength, flexural strength and rigidity of the PPS composite material.
[0014] Preferably, the preparation method of the modified PPS resin includes the following steps:
[0015] (R1) Place the PPS resin at the downwind of the PECVD reaction chamber. After evacuating the PECVD reaction chamber, add glycidyl methacrylate and continuously introduce oxygen, control the pressure in the PECVD reaction chamber at 12 - 15 Pa, and the reaction temperature at 40 - 60 °C;
[0016] (R2) Under the action of an excitation source, oxygen is excited into plasma to initiate the graft polymerization reaction of glycidyl methacrylate and PPS resin. Stop the action of the excitation source and stop introducing oxygen. After cooling to room temperature, the modified PPS resin is obtained.
[0017] With the above technical solution, oxygen is excited into plasma by plasma enhanced chemical vapor deposition (PECVD), and then the PPS resin is subjected to plasma surface treatment. The active free radicals generated on the surface are used to initiate graft copolymerization of glycidyl methacrylate on the surface of the PPS resin, increasing the active groups of the PPS resin and improving the adhesion to epoxy resin.
[0018] Preferably, the weight average molecular weight of the PPS resin is 20,000 - 50,000; the weight ratio of the PPS resin to glycidyl methacrylate is 100:10 - 20.
[0019] With the above technical solution, the PPS resin with a weight average molecular weight of 20,000 - 50,000 has a lower viscosity, better dispersion effect on glass fiber and filler, which is beneficial to improving the surface smoothness of the PPS composite material and enhancing the quality.
[0020] Preferably, the excitation source is radio frequency, DC high voltage, pulse or microwave, the output power of the excitation source is 200 - 300W, and the reaction time is 1 - 2h.
[0021] With the above technical solution, it promotes the excitation of oxygen into plasma and the cathode to generate glow discharge or high-frequency discharge. More preferably, the excitation source is radio frequency, specifically an inductively coupled plasma radio frequency power supply is used to generate the excitation source. By controlling the output power of the excitation source at 200 - 300W, the reaction process is fully absorbed, so as to ensure that the reflected power of the excitation source only reaches 0 - 30W and the effective power is high; in addition, by controlling the output power of the excitation source at 200 - 300W, the plasma has stronger activity and higher processing efficiency under this power condition; if the output power of the excitation source is too high, due to excessive energy absorption of the PPS resin, it is easy to damage the molecular structure of the PPS resin and cause its degradation. The reaction time is controlled at 1 - 2h to fully modify the PPS resin.
[0022] Preferably, the filler is talcum powder or silica; the coupling agent is KH560 or KH580.
[0023] With the above technical solution, talcum powder or silica can form siloxane bonds with certain adhesion to epoxy resin, so it is more beneficial to increase the adhesion during the adhesion process with epoxy. The addition of KH560 or KH580 greatly improves the mechanical properties. The main reason is that the added coupling agent improves the compatibility of the system. In addition, due to the coupling agent having more active groups, it can also enhance the adhesion between the PPS composite material and epoxy resin.
[0024] Preferably, the chain extender is ethylene - maleic anhydride copolymer, the weight average molecular weight of the ethylene - maleic anhydride copolymer is 8000 - 12000; the antioxidant is S9228; the other additive is color powder.
[0025] By adopting the above technical solution, the added ethylene-maleic anhydride copolymer links the molecular chains of the raw materials, reduces the breakage caused by thermal degradation during processing, and increases the molecular connection points of the raw materials, provides more active groups, and improves the bonding effect. The antioxidant S9228 used has excellent high temperature stability and low volatility at high temperatures. It can maintain excellent hydrolysis stability even when exposed to a humid environment, which is beneficial to improve the high temperature and high humidity resistance of the PPS composite material.
[0026] The second object of the present invention is achieved by the following technical solution: The method for preparing the above-mentioned high-adhesion PPS composite material comprises the following steps:
[0027] (S1), taking each raw material by weight and setting aside;
[0028] (S2) premixing the modified PPS resin and the coupling agent in a high-speed mixer for 2 minutes, adding a toughening agent, a chain extender, an antioxidant and other additives and mixing for 2 minutes before discharging the mixture into a twin-screw extruder. The glass fiber and the filler are respectively fed into the twin-screw extruder at two strong sides, and extruded and granulated under a screw combination of a certain shear strength to obtain a high-adhesion PPS composite material.
[0029] Among them, the processing temperatures of each section of the twin-screw extruder starting from the feeding section are respectively: 200°C, 290°C, 290°C, 290°C, 290°C, 290°C, 290°C, 290°C, 290°C, 290°C, the head temperature is 295°C, and the screw speed is 360 r / min; moreover, the screw combination successively includes the following elements from the head to the tail: 32 / 32A, 48 / 48, 48 / 48, 48 / 48, 48 / 48, 32 / 32, 32 / 32, 22 / 22, 22 / 22, 22 / 22, K30° / 7 / 48, K45° / 5 / 32, K60° / 4 / 22, 32 / 32, 22 / 22, 22 / 22, 22 / 22, K60° / 4 / 22, K90° / 5 / 32, 22 / 11L, 48 / 48, 48 / 48, 48 / 48, 32 / 32, 22 / 22, 22 / 22, K45° / 5 / 32, K60° / 4 / 22, 32 / 32, 22 / 22, 22 / 22, ZME gasket, ZME22 / 22, ZME22 / 22, ZME gasket, 48 / 48, 48 / 48, 48 / 48, 32 / 32, 32 / 32, 32 / 32, 32 / 32, 22 / 22, and the length of the screw combination is 1450 - 1500 mm; among them, a main feeding and discharging port is arranged at the second element of the screw combination, a filler strong-side feeding port is arranged at the third element of the screw combination, and a glass fiber strong-side feeding port is arranged at the 26th element of the screw combination. The main use of the screw combination is to fill the filler from the second-stage strong-side feeding, which is beneficial to the uniform addition of the filler and solves the problem of powder accumulation at the feeding port; in addition, the toothed disc of ZME is beneficial to the dispersion of the material, strengthens the dispersion of the material, promotes the synergistic effect of each raw material of the PPS composite material, improves the epoxy bonding force and mechanical properties, and is beneficial to the strip forming and performance uniformity after the material is uniform.
[0030] The third object of the present invention is achieved by the following technical solution: An application of a high-adhesion PPS composite material in a capacitor housing, and the high-adhesion PPS composite material is used as a base material for producing a capacitor housing.
[0031] The beneficial effects of the present invention are as follows: The high-adhesion PPS composite material of the present invention uses a modified PPS resin as the main material, and a toughening agent, glass fiber, filler, coupling agent, chain extender, antioxidant and other additives are added to further blend and modify the modified PPS resin. Through their synergistic effects, its toughness is improved, chain breakage is reduced, more excellent mechanical properties are obtained, more active groups are provided, the bonding force with epoxy resin is enhanced, the problem of easy peeling off when bonded with epoxy resin is avoided, and it is beneficial to maintain a high tightness with epoxy resin.
[0032] The preparation method of the high-adhesion PPS composite material of the present invention is simple to operate, convenient to control, has high production efficiency and low production cost, and can be used for large-scale production.
[0033] The application of the high-adhesion PPS composite material of the present invention in the capacitor housing. The high-adhesion PPS composite material is used as the base material for producing the capacitor housing, and has excellent comprehensive properties. At the same time, it has good high-temperature and high-humidity resistance characteristics. After testing for 1000 hours under the conditions of 85% humidity and 85 °C, the epoxy bond strength on the surface is still very strong. Detailed implementation manners
[0034] For the convenience of understanding by those skilled in the art, the present invention will be further described below in conjunction with embodiments. The content mentioned in the implementation manners does not limit the present invention.
[0035] Embodiment 1
[0036] A high-adhesion PPS composite material, comprising the following raw materials in parts by weight:
[0037]
[0038] The toughening agent is SEBS-g-MAH (FG1901).
[0039] The glass fiber is high-modulus chopped glass fiber, with an elastic modulus of 94.0 GPa and a chopped length of 3.5 mm.
[0040] The preparation method of the modified PPS resin comprises the following steps:
[0041] (R1), Place the PPS resin at the downwind of the PECVD reaction chamber. After evacuating the PECVD reaction chamber, add glycidyl methacrylate and continuously introduce oxygen, control the pressure in the PECVD reaction chamber at 13 Pa, and the reaction temperature at 50 °C;
[0042] (R2), Under the action of the excitation source, oxygen is excited into plasma and the graft polymerization reaction of glycidyl methacrylate and PPS resin is initiated. Stop the action of the excitation source and stop introducing oxygen. After cooling to room temperature, the modified PPS resin is obtained.
[0043] The weight-average molecular weight of the PPS resin is 2W; the weight ratio of the PPS resin to glycidyl methacrylate is 100:15.
[0044] The excitation source is radio frequency, the output power of the excitation source is 250 W, and the reaction time is 1.5 h.
[0045] The filler is talcum powder; the coupling agent is KH560.
[0046] The chain extender is ethylene - maleic anhydride copolymer, and the weight - average molecular weight of the ethylene - maleic anhydride copolymer is 10,000.
[0047] The preparation method of the high - adhesion PPS composite material includes the following steps:
[0048] (S1) Weigh each raw material by weight parts and set aside.
[0049] (S2) Premix the modified PPS resin and the coupling agent in a high - speed mixer for 2 min, then add the toughening agent, chain extender, antioxidant and other additives, mix for 2 min and then discharge to a twin - screw extruder. The glass fiber and the filler are respectively fed into the twin - screw extruder through two strong side - feeding devices, and granulation is carried out under the condition of a screw combination with a certain shear strength to obtain the high - adhesion PPS composite material.
[0050] Among them, the processing temperatures of each section of the twin - screw extruder from the feeding section are: 200 °C, 290 °C, 290 °C, 290 °C, 290 °C, 290 °C, 290 °C, 290 °C, 290 °C, 290 °C, and the head temperature is 295 °C, and the screw speed is 360 r / min; moreover, the screw combination includes the following elements in sequence from the head to the tail: 32 / 32A, 48 / 48, 48 / 48, 48 / 48, 48 / 48, 32 / 32, 32 / 32, 22 / 22, 22 / 22, 22 / 22, K30° / 7 / 48, K45° / 5 / 32, K60° / 4 / 22, 32 / 32, 22 / 22, 22 / 22, 22 / 22, K60° / 4 / 22, K90° / 5 / 32, 22 / 11L, 48 / 48, 48 / 48, 48 / 48, 32 / 32, 22 / 22, 22 / 22, K45° / 5 / 32, K60° / 4 / 22, 32 / 32, 22 / 22, 22 / 22, ZME gasket, ZME22 / 22, ZME22 / 22, ZME gasket, 48 / 48, 48 / 48, 48 / 48, 32 / 32, 32 / 32, 32 / 32, 32 / 32, 22 / 22, and the length of the screw combination is 1485.5 mm; among them, the main feeding hopper is set at the second element of the screw combination, the strong side - feeding port for the filler is set at the third element of the screw combination, and the strong side - feeding port for the glass fiber is set at the 26th element of the screw combination.
[0051] Example 2
[0052] A high - adhesion PPS composite material, comprising the following raw materials by weight parts:
[0053]
[0054]
[0055] The toughening agent is POE-g-GMA (SOG-02).
[0056] The glass fiber is high-modulus chopped glass fiber with an elastic modulus of 93.0 GPa and a chopped length of 2.0 mm.
[0057] The preparation method of the modified PPS resin includes the following steps:
[0058] (R1) Place the PPS resin at the downwind of the PECVD reaction chamber. After evacuating the PECVD reaction chamber, add glycidyl methacrylate and continuously introduce oxygen. Control the pressure in the PECVD reaction chamber at 12 Pa and the reaction temperature at 40 °C;
[0059] (R2) Under the action of the excitation source, oxygen is excited into plasma to initiate the graft polymerization reaction of glycidyl methacrylate and PPS resin. Stop the action of the excitation source and stop introducing oxygen. After cooling to room temperature, the modified PPS resin is obtained.
[0060] The weight-average molecular weight of the PPS resin is 50,000; the weight ratio of the PPS resin to glycidyl methacrylate is 100:10.
[0061] The excitation source is radio frequency, the output power of the excitation source is 200 W, and the reaction time is 1 h.
[0062] The filler is talcum powder; the coupling agent is KH560.
[0063] The chain extender is ethylene-maleic anhydride copolymer, and the weight-average molecular weight of the ethylene-maleic anhydride copolymer is 8,000.
[0064] The preparation method of the high-adhesion PPS composite material includes the following steps:
[0065] (S1) Weigh each raw material by weight and set aside;
[0066] (S2) Premix the modified PPS resin and the coupling agent in a high-speed mixer for 2 min, then add the toughening agent, chain extender, antioxidant and other additives, mix for 2 min and then discharge to a twin-screw extruder. The glass fiber and the filler are respectively fed into the twin-screw extruder through two strong side feeds, and pelletized under the condition of a screw combination with a certain shear strength to obtain the high-adhesion PPS composite material.
[0067] Among them, the processing temperatures of each section of the twin-screw extruder starting from the feeding section are: 200°C, 290°C, 290°C, 290°C, 290°C, 290°C, 290°C, 290°C, 290°C, 290°C, the head temperature is 295°C, and the screw speed is 360 r / min; moreover, the screw combination successively includes the following elements from the head to the tail: 32 / 32A, 48 / 48, 48 / 48, 48 / 48, 48 / 48, 32 / 32, 32 / 32, 22 / 22, 22 / 22, 22 / 22, K30° / 7 / 48, K45° / 5 / 32, K60° / 4 / 22, 32 / 32, 22 / 22, 22 / 22, 22 / 22, K60° / 4 / 22, K90° / 5 / 32, 22 / 11L, 48 / 48, 48 / 48, 48 / 48, 32 / 32, 22 / 22, 22 / 22, K45° / 5 / 32, K60° / 4 / 22, 32 / 32, 22 / 22, 22 / 22, ZME gasket, ZME22 / 22, ZME22 / 22, ZME gasket, 48 / 48, 48 / 48, 48 / 48, 32 / 32, 32 / 32, 32 / 32, 32 / 32, 22 / 22, and the length of the screw combination is 1485.5 mm; among them, the main feeding hopper is arranged at the second element of the screw combination, the filler strong-side feeding port is arranged at the third element of the screw combination, and the glass fiber strong-side feeding port is arranged at the 26th element of the screw combination.
[0068] Example 3
[0069] A high-adhesion PPS composite material comprises the following raw materials in parts by weight:
[0070]
[0071] The toughening agent is SEBS-g-MAH (FG1901).
[0072] The glass fiber is high-modulus chopped glass fiber with an elastic modulus of 95.0 GPa and a chopped length of 4.5 mm.
[0073] The preparation method of the modified PPS resin comprises the following steps:
[0074] (R1), Place the PPS resin at the downwind of the PECVD reaction chamber. After evacuating the PECVD reaction chamber, add glycidyl methacrylate and continuously introduce oxygen, control the pressure in the PECVD reaction chamber at 15 Pa, and the reaction temperature at 60°C;
[0075] (R2) Under the action of an excitation source, oxygen is excited into a plasma, and the graft polymerization reaction of glycidyl methacrylate and PPS resin is initiated. After stopping the action of the excitation source and stopping the supply of oxygen, and cooling to room temperature, the modified PPS resin is obtained.
[0076] The weight-average molecular weight of the PPS resin is 30,000; the weight ratio of the PPS resin to glycidyl methacrylate is 100:20.
[0077] The excitation source is radio frequency, the output power of the excitation source is 300 W, and the reaction time is 2 h.
[0078] The filler is silica; the coupling agent is KH580.
[0079] The chain extender is an ethylene-maleic anhydride copolymer, and the weight-average molecular weight of the ethylene-maleic anhydride copolymer is 12,000.
[0080] The preparation method of the high-adhesion PPS composite material includes the following steps:
[0081] (S1) Weigh each raw material by weight and set aside.
[0082] (S2) Premix the modified PPS resin and the coupling agent in a high-speed mixer for 2 min, then add the toughening agent, chain extender, antioxidant and other additives, mix for 2 min, and then discharge to a twin-screw extruder. The glass fiber and the filler are respectively fed into the twin-screw extruder through two strong side feeders, and pelletized by extrusion under the condition of a screw combination with a certain shear strength to obtain the high-adhesion PPS composite material.
[0083] Among them, the processing temperatures of each section of the twin-screw extruder starting from the feeding section are respectively: 200°C, 290°C, 290°C, 290°C, 290°C, 290°C, 290°C, 290°C, 290°C, 290°C, the head temperature is 295°C, and the screw speed is 360 r / min; moreover, the screw combination successively includes the following elements from the head to the tail: 32 / 32A, 48 / 48, 48 / 48, 48 / 48, 48 / 48, 32 / 32, 32 / 32, 22 / 22, 22 / 22, 22 / 22, K30° / 7 / 48, K45° / 5 / 32, K60° / 4 / 22, 32 / 32, 22 / 22, 22 / 22, 22 / 22, K60° / 4 / 22, K90° / 5 / 32, 22 / 11L, 48 / 48, 48 / 48, 48 / 48, 32 / 32, 22 / 22, 22 / 22, K45° / 5 / 32, K60° / 4 / 22, 32 / 32, 22 / 22, 22 / 22, ZME gasket, ZME22 / 22, ZME22 / 22, ZME gasket, 48 / 48, 48 / 48, 48 / 48, 32 / 32, 32 / 32, 32 / 32, 32 / 32, 22 / 22, and the length of the screw combination is 1485.5 mm; among them, a main feeding and discharging port is arranged at the second element of the screw combination, a filler strong-side feeding port is arranged at the third element of the screw combination, and a glass fiber strong-side feeding port is arranged at the 26th element of the screw combination.
[0084] Example 4
[0085] A high-adhesion PPS composite material comprises the following raw materials in parts by weight:
[0086]
[0087] The toughening agent is ethylene-methyl acrylate copolymer EMA (1209AC).
[0088] The glass fiber is high-modulus chopped glass fiber with an elastic modulus of 94.0 GPa and a chopped length of 2.5 mm.
[0089] The preparation method of the modified PPS resin comprises the following steps:
[0090] (R1), Place the PPS resin at the lower air inlet of the PECVD reaction chamber, evacuate the PECVD reaction chamber and then add glycidyl methacrylate and continuously introduce oxygen, control the pressure in the PECVD reaction chamber at 14 Pa, and the reaction temperature at 48°C;
[0091] (R2) Under the action of an excitation source, oxygen is excited into a plasma, and a graft polymerization reaction of glycidyl methacrylate and PPS resin is initiated. After stopping the action of the excitation source and stopping the supply of oxygen, and cooling to room temperature, a modified PPS resin is obtained.
[0092] The weight-average molecular weight of the PPS resin is 40,000; the weight ratio of the PPS resin to glycidyl methacrylate is 100:18.
[0093] The excitation source is radio frequency, the output power of the excitation source is 280 W, and the reaction time is 1.8 h.
[0094] The filler is talcum powder; the coupling agent is KH560.
[0095] The chain extender is an ethylene-maleic anhydride copolymer, and the weight-average molecular weight of the ethylene-maleic anhydride copolymer is 10,000.
[0096] The preparation method of the high-adhesion PPS composite material includes the following steps:
[0097] (S1) Weigh each raw material by weight and set aside.
[0098] (S2) Premix the modified PPS resin and the coupling agent in a high-speed mixer for 2 min, then add the toughening agent, chain extender, antioxidant and other additives, mix for 2 min, and then discharge to a twin-screw extruder. The glass fiber and the filler are respectively fed into the twin-screw extruder through two strong side feeders, and granulation is carried out under the condition of a screw combination with a certain shear strength to obtain a high-adhesion PPS composite material.
[0099] Among them, the processing temperatures of each section of the twin-screw extruder starting from the feeding section are respectively: 200°C, 290°C, 290°C, 290°C, 290°C, 290°C, 290°C, 290°C, 290°C, 290°C, the head temperature is 295°C, and the screw speed is 360 r / min; moreover, the screw combination includes the following elements in sequence from the head to the tail of the machine: 32 / 32A, 48 / 48, 48 / 48, 48 / 48, 48 / 48, 32 / 32, 32 / 32, 22 / 22, 22 / 22, 22 / 22, K30° / 7 / 48, K45° / 5 / 32, K60° / 4 / 22, 32 / 32, 22 / 22, 22 / 22, 22 / 22, K60° / 4 / 22, K90° / 5 / 32, 22 / 11L, 48 / 48, 48 / 48, 48 / 48, 32 / 32, 22 / 22, 22 / 22, K45° / 5 / 32, K60° / 4 / 22, 32 / 32, 22 / 22, 22 / 22, ZME gasket, ZME22 / 22, ZME22 / 22, ZME gasket, 48 / 48, 48 / 48, 48 / 48, 32 / 32, 32 / 32, 32 / 32, 32 / 32, 22 / 22, and the length of the screw combination is 1485.5 mm; among them, a main feeding hopper is arranged at the second element of the screw combination, a filler strong-side feeding port is arranged at the third element of the screw combination, and a glass fiber strong-side feeding port is arranged at the 26th element of the screw combination.
[0100] Comparative Example 1
[0101] A high-adhesion PPS composite material, comprising the following raw materials in parts by weight:
[0102]
[0103] The toughening agent is SEBS-g-MAH (FG1901).
[0104] The glass fiber is high-modulus chopped glass fiber with an elastic modulus of 94.0 GPa and a chopped length of 3.5 mm.
[0105] The weight-average molecular weight of the PPS resin is 2W.
[0106] The filler is talc powder; the coupling agent is KH560.
[0107] The chain extender is ethylene-maleic anhydride copolymer, and the weight-average molecular weight of the ethylene-maleic anhydride copolymer is 10,000.
[0108] The preparation method of the high-adhesion PPS composite material includes the following steps:
[0109] (S1), take each raw material according to parts by weight and set aside;
[0110] (S2) Premix the modified PPS resin and the coupling agent in a high-speed mixer for 2 min, then add the toughening agent, chain extender, antioxidant and other additives, mix for 2 min and discharge to a twin-screw extruder. The glass fiber and filler are fed into the twin-screw extruder through two strong side feeders respectively, and pelletize by extrusion under the condition of a screw combination with a certain shear strength to obtain a PPS composite with high adhesion force.
[0111] Among them, the processing temperatures of each section of the twin-screw extruder starting from the feeding section are: 200 °C, 290 °C, 290 °C, 290 °C, 290 °C, 290 °C, 290 °C, 290 °C, 290 °C, 290 °C, and the head temperature is 295 °C, and the screw speed is 360 r / min; moreover, the screw combination includes the following elements in sequence from the head to the tail: 32 / 32A, 48 / 48, 48 / 48, 48 / 48, 48 / 48, 32 / 32, 32 / 32, 22 / 22, 22 / 22, 22 / 22, K30° / 7 / 48, K45° / 5 / 32, K60° / 4 / 22, 32 / 32, 22 / 22, 22 / 22, 22 / 22, K60° / 4 / 22, K90° / 5 / 32, 22 / 11L, 48 / 48, 48 / 48, 48 / 48, 32 / 32, 22 / 22, 22 / 22, K45° / 5 / 32, K60° / 4 / 22, 32 / 32, 22 / 22, 22 / 22, ZME gasket, ZME22 / 22, ZME22 / 22, ZME gasket, 48 / 48, 48 / 48, 48 / 48, 32 / 32, 32 / 32, 32 / 32, 32 / 32, 22 / 22, and the length of the screw combination is 1485.5 mm; among them, the main feeding discharge port is arranged at the second element of the screw combination, the filler strong side feeding port is arranged at the third element of the screw combination, and the glass fiber strong side feeding port is arranged at the 26th element of the screw combination.
[0112] Comparative Example 2
[0113] The difference between this comparative example and Example 1 is that:
[0114] The chain extender is replaced with an epoxy modifier (bisphenol A epoxy resin E-44).
[0115] Comparative Example 3
[0116] The difference between this comparative example and Example 1 is that:
[0117] The filler is wollastonite.
[0118] Comparative Example 4
[0119] The difference between this comparative example and Example 1 is that:
[0120] The screw combination successively includes the following elements from the head to the tail of the machine head: 32 / 32A, 48 / 48, 48 / 48, 48 / 48, 48 / 48, 32 / 32, 32 / 32, 22 / 22, 22 / 22, 22 / 22, K30° / 7 / 48, K45° / 5 / 32, K60° / 4 / 22, 32 / 32, 22 / 22, 22 / 22, 22 / 22, K60° / 4 / 22, K90° / 5 / 32, 22 / 11L, 48 / 48, 48 / 48, 48 / 48, 32 / 32, 22 / 22, 22 / 22, K45° / 5 / 32, K60° / 4 / 22, 32 / 32, 22 / 22, 22 / 22, 22 / 22, 22 / 22, 22 / 22, 22 / 22, 48 / 48, 48 / 48, 48 / 48, 32 / 32, 32 / 32, 32 / 32, 32 / 32, 22 / 22. The length of the screw combination is 1485.5 mm. Among them, a main feeding discharge port and a filler strong side feeding port are arranged at the second element of the screw combination, and a glass fiber strong side feeding port is arranged at the 26th element of the screw combination.
[0121] Comparative Example 5
[0122] A PPS resin, the weight average molecular weight of the PPS resin is 2W.
[0123] Performance test
[0124] Take the PPS composites of Examples 1-4 and Comparative Examples 1-5, and respectively test their non-notched impact strength, notched impact strength, tensile strength, flexural strength, and epoxy adhesion after treatment under double 85 conditions. The test methods are as follows:
[0125] Non-notched impact strength: According to the determination of plastic impact strength in ISO-180, perform non-notched impact test;
[0126] Notched impact strength: According to the determination of plastic impact strength in ISO-180, perform notched impact test;
[0127] Tensile strength: According to the determination of plastic tensile properties in ISO-527, perform tensile strength test;
[0128] Flexural strength: According to the determination of plastic flexural properties in ISO 178, perform flexural strength test;
[0129] Epoxy adhesion after treatment under double 85 conditions: Take dumbbell-shaped specimens. After being treated under the conditions of 85% humidity and 85 °C for 1000 hours, cut them into 2 sections from the middle of the dumbbell. Select the reverse side of the 20 mm length of the same spline thimble mark from the fracture for gluing (wipe the surface with alcohol before gluing). Bonding area: 20 mm (length) x 10 mm (width) = 200 mm2 , then, a layer of epoxy resin curing agent mixture is evenly coated on the surface with a cotton swab, and fixed at the bonding part with a long-tail clip (the types and sizes of the long-tail clips are the same). Then, the epoxy resin is cured in an oven (curing conditions: 120 °C, 2 hours). After cooling for 24 hours, the sample is ready for testing. The shear tensile strength is tested with a universal testing machine according to GB / T 1040.1-2006, the testing speed is 5 mm / min, and the unit is MPa.
[0130] The test results are shown in the following table:
[0131]
[0132]
[0133] As can be seen from the above table, the high-adhesion PPS composite material of the present invention, as the base material for producing the capacitor housing, has excellent comprehensive properties, and at the same time has good high-temperature and high-humidity characteristics. After testing for 1000 hours under the conditions of 85% humidity and 85 °C, the surface epoxy adhesion is still very strong.
[0134] The above embodiments are the preferred implementation schemes of the present invention. In addition, the present invention can also be implemented in other ways. Any obvious replacement without departing from the concept of the present invention is within the protection scope of the present invention.
Claims
1. A high-adhesion PPS composite material, characterized in that: It comprises the following raw materials in parts by weight: Modified PPS resin 40 - 60 parts Toughening agent 1 - 10 parts Glass fiber 20 - 40 parts Filler 10 - 30 parts Coupling agent 1 - 5 parts Chain extender 0.1 - 0.5 part Antioxidant 0.1 - 0.2 part Other additives 0.5 - 1.0 part; The preparation method of the modified PPS resin comprises the following steps: (R1), Place the PPS resin at the downwind of the PECVD reaction chamber. After evacuating the PECVD reaction chamber, add glycidyl methacrylate and continuously introduce oxygen. Control the pressure in the PECVD reaction chamber at 12 - 15 Pa, and the reaction temperature at 40 - 60 °C; (R2), Under the action of an excitation source, oxygen is excited into plasma and initiates the graft polymerization reaction of glycidyl methacrylate and PPS resin. Stop the action of the excitation source and stop introducing oxygen. After cooling to room temperature, the modified PPS resin is obtained.
2. A high-adhesion PPS composite material according to claim 1, characterized in that: The toughening agent is at least one of POE-g-GMA, ethylene-butyl acrylate copolymer EBA, ethylene-methyl acrylate copolymer EMA or SEBS-g-MAH.
3. A high-adhesion PPS composite material according to claim 1, characterized in that: The glass fiber is high-modulus chopped glass fiber.
4. A high-adhesion PPS composite material according to claim 1, characterized in that: The weight-average molecular weight of the PPS resin is 20,000 - 50,000; the weight ratio of the PPS resin to glycidyl methacrylate is 100:10 - 20.
5. A high-adhesion PPS composite material according to claim 4, characterized in that: The excitation source is radio frequency, DC high voltage, pulse or microwave, the output power of the excitation source is 200 - 300 W, and the reaction time is 1 - 2 h.
6. A high-adhesion PPS composite material according to claim 1, characterized in that: The filler is talc powder or silica; the coupling agent is KH560 or KH580.
7. A high-adhesion PPS composite material according to claim 1, characterized in that: The chain extender is ethylene-maleic anhydride copolymer, and the weight-average molecular weight of the ethylene-maleic anhydride copolymer is 8000 - 12000; the antioxidant is S9228; the other additives are color powder.
8. A preparation method of a high-adhesion PPS composite material according to any one of claims 1 - 7, characterized in that it comprises the following steps: (S1), Weigh each raw material according to parts by weight and set aside; (S2), Premix the modified PPS resin and the coupling agent in a high-speed mixer for 2 min, then add the toughening agent, chain extender, antioxidant and other additives, mix for 2 min and then discharge to a twin-screw extruder. The glass fiber and the filler are respectively fed into the twin-screw extruder through two strong side feeders, and granulation is carried out under the condition of a screw combination with a certain shear strength to obtain the high-adhesion PPS composite material.
9. Application of the high-adhesion PPS composite material according to any one of claims 1-7 in a capacitor housing, characterized in that: the high-adhesion PPS composite material is used as a base material for producing a capacitor housing.
Citation Information
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