WO2018137320A1 - Matière première de ferrule mt et procédé de préparation associé - Google Patents

Matière première de ferrule mt et procédé de préparation associé Download PDF

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Publication number
WO2018137320A1
WO2018137320A1 PCT/CN2017/093166 CN2017093166W WO2018137320A1 WO 2018137320 A1 WO2018137320 A1 WO 2018137320A1 CN 2017093166 W CN2017093166 W CN 2017093166W WO 2018137320 A1 WO2018137320 A1 WO 2018137320A1
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Prior art keywords
raw material
ferrule
mass percentage
ferrule raw
antioxidant
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PCT/CN2017/093166
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English (en)
Chinese (zh)
Inventor
黄雪云
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潮州三环（集团）股份有限公司
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Publication of WO2018137320A1 publication Critical patent/WO2018137320A1/fr

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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
    • C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/92—Measuring, controlling or regulating
    • 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
    • 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
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/92704—Temperature
    • 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
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • 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
    • C08K2003/2244—Oxides; Hydroxides of metals of zirconium
    • 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
    • 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
    • C08K2003/2296—Oxides; Hydroxides of metals of zinc
    • 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
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C08K2003/265—Calcium, strontium or barium carbonate

Definitions

  • the invention relates to a communication technology, in particular to an MT ferrule raw material and a preparation method thereof.
  • Polyphenylene sulfide is a special engineering plastic with excellent comprehensive performance. It has high temperature resistance, corrosion resistance, radiation resistance, non-combustibility, non-toxicity, excellent mechanical and electrical properties, good dimensional stability of products, and various methods. Forming processing and secondary processing of the product. Polyphenylene sulfide resin has low melt viscosity, can mix a large amount of filler material, and has low molding shrinkage. This material can be used to obtain MT ferrules with high dimensional accuracy, and the obtained MT ferrule has low water absorption rate and small dimensional change after water absorption. , good chemical resistance and good dimensional stability. However, the rigid structure of the polyphenylene sulfide resin determines its superior performance, and also makes its disadvantage, brittleness, extremely obvious.
  • the raw materials applied to the MT ferrule are mainly PPS (polyphenylene sulfide) and SiO 2 microspheres.
  • PPS polyphenylene sulfide
  • SiO 2 microspheres By adding SiO 2 microspheres, the dimensional stability of the material is ensured and the strength is enhanced.
  • the commonly used preparation methods of SiO 2 microspheres generally require the use of a large amount of organic matter, which is troublesome to recycle, high in cost and environmentally polluted, and requires high equipment, complicated operation, and high energy consumption, and is suitable for existing MT ferrule raw materials.
  • the invention has the advantages that the improved inorganic filler and the optimization of the preparation process enable the prepared MT ferrule raw material to have better dimensional stability, lower thermal expansion coefficient, lower preparation cost and longer service life.
  • the object of the present invention is to overcome the above-mentioned deficiencies of the prior art and to provide an MT ferrule raw material which can reduce cost, simplify the process and improve stability, and a preparation method thereof.
  • the technical solution adopted by the present invention is: an MT ferrule raw material, the ferrule raw material comprising the following components according to a mass percentage: 14.5-35% polyphenylene sulfide, and 55-85%
  • the inorganic filler is at least one of zirconium dioxide, silicon dioxide, aluminum oxide, iron oxide, zinc oxide, and calcium carbonate.
  • the ferrule raw material further contains 0.1 to 2% of a coupling agent in terms of mass percentage.
  • the coupling agent is used for modifying the inorganic filler, and is modified by the coupling agent to make the PPS and the filler microspheres better connected together, reducing the dropping rate of the filler microspheres and increasing the strength of the material.
  • the coupling agent comprises vinyl silane, stearic acid amide, ⁇ -glyceryloxypropyltrimethoxysilane, ⁇ -methacryloyloxytrimethoxysilane, ⁇ -mercaptopropyltrimethyl At least one of oxysilane and 3-propyl methacrylate trimethoxysilane.
  • the inorganic filler is at least one of zirconium dioxide and aluminum oxide.
  • the inorganic filler is at least one of calcium carbonate and aluminum oxide.
  • the inventors of the present application have found through repeated tests that when the inorganic filler is selected from calcium carbonate or/and alumina, the impact strength of the obtained MT ferrule raw material is significantly higher than that of other fillers.
  • the polyphenylene sulfide has a mass percentage of 21 to 26%.
  • the inorganic filler has a mass percentage of 57 to 67%.
  • the component of the ferrule raw material further comprises a stabilizer having a mass percentage of 0 to 30%; more preferably, the stabilizer has a mass percentage of 0.17 to 14.4%; most preferably, The mass percentage of the stabilizer is from 1.2 to 3%.
  • the stabilizer is selected from at least one of a lead salt, a metal soap, an organic rare earth, and an organotin.
  • the lead salt may be a tribasic lead sulfate or a dibasic lead phosphite;
  • the metal soap may be lead stearate, lead 2-ethyl acetate, barium stearate, cadmium stearate or stearic acid.
  • the organic rare earth may be a carboxylate or a fatty acid salt of a light rare earth element such as lanthanum, cerium, lanthanum or cerium
  • the organotin may be tin isooctyl dimethyl dimercaptoacetate or isooctyl dimercaptoacetate Octyl tin, di-n-butyltin dilaurate or di-n-octyltin dilaurate.
  • the component of the ferrule raw material further comprises a plasticizer having a mass percentage of 0 to 30%; more preferably, the plasticizer has a mass percentage of 0.1 to 8.3%; Preferably, the plasticizer The mass percentage is from 1 to 3.5%.
  • the plasticizer is at least one of di(2-ethylhexyl) phthalate, DINP, DNOP, DBP, DMP and DEP.
  • DINP is diisodecyl phthalate
  • DNOP is di-n-octyl phthalate
  • DBP is dibutyl phthalate
  • DMP is dimethyl phthalate
  • DEP is N, N- Diethylpropynylamine.
  • the component of the ferrule raw material further comprises an antioxidant having a mass percentage of 0 to 30%; more preferably, the antioxidant has a mass percentage of 0.13 to 13.5%; most preferably, The antioxidant has a mass percentage of 1.9 to 7%.
  • the antioxidant is at least one of 2,6-di-tert-butyl-4-methylphenol, antioxidant 2246, antioxidant 1010, thiodipropionate, and thiophosphite.
  • the thiodipropionate may be dilauryl thiodipropionate; the thiophosphite may be triphenyl thiophosphite.
  • the present invention also provides a method for preparing the above MT ferrule raw material, comprising the following steps:
  • step b adding a coupling agent to the uniformly dispersed inorganic filler organic solution obtained in the step a, and simultaneously treating with the second ultrasonication by the second high-speed stirring, and drying, the filler microspheres can be obtained;
  • the filler microspheres obtained in the step (1) are premixed with polyphenylene sulfide, and then melt blended into a twin-screw extruder to obtain a composite material in which the filler microspheres are uniformly dispersed in the polyphenylene sulfide resin matrix, and the composite is obtained.
  • the material is the MT ferrule raw material.
  • the inorganic filler in the step (1) is at least one of zirconium dioxide, silicon dioxide, aluminum oxide, iron oxide, zinc oxide and calcium carbonate. It should be noted that the inventors of the present application have found through experiments that when the inorganic filler in the step (1) is a micron-sized zirconium dioxide particle, the obtained MT material is the most stable, has the lowest thermal expansion coefficient and the highest strength; The spherical particles of zirconium dioxide are easy to control the morphology and have a large specific surface area, which is favorable for subsequent surface modification by a coupling agent.
  • the organic solvent in the step (1) includes at least one of methanol, ethanol, propanol, acetone, toluene, and N-methylpyrrolidone.
  • the coupling agent in the step (1) comprises vinyl silane, stearic acid amide, ⁇ -glyceryloxypropyltrimethoxysilane, ⁇ -methacryloyloxytrimethoxysilane, ⁇ At least one of mercaptopropyltrimethoxysilane and 3-propyl methacrylatetrimethoxysilane.
  • step b at least one of a stabilizer, a plasticizer and an antioxidant is further added to the uniformly dispersed inorganic filler organic solution obtained in the step a.
  • the stabilizer is selected from at least one of a lead salt, a metal soap, an organic rare earth, and an organotin.
  • the lead salt may be a tribasic lead sulfate or a dibasic lead phosphite;
  • the metal soap may be lead stearate, lead 2-ethyl acetate, barium stearate, cadmium stearate or stearic acid.
  • the organic rare earth may be a carboxylate or a fatty acid salt of a light rare earth element such as lanthanum, cerium, lanthanum or cerium
  • the organotin may be tin isooctyl dimethyl dimercaptoacetate or isooctyl dimercaptoacetate Octyl tin, di-n-butyltin dilaurate or di-n-octyltin dilaurate.
  • the plasticizer is at least one of di(2-ethylhexyl) phthalate, DINP, DNOP, DBP, DMP and DEP.
  • the antioxidant is at least one of 2,6-di-tert-butyl-4-methylphenol, antioxidant 2246, antioxidant 1010, thiodipropionate and thiophosphite.
  • the thiodipropionate may be dilauryl thiodipropionate; the thiophosphite may be triphenyl thiophosphite.
  • the stabilizer, the plasticizer, and the antioxidant are each 0 to 30% by mass; more preferably, the stabilizer has a mass percentage of 0.17 to 14.4%; the plasticizing The mass percentage of the agent is 0.1 to 8.3%; the mass percentage of the antioxidant is 0.13 to 13.5%; most preferably, the mass percentage of the stabilizer is 1.2 to 3%; The mass percentage of the agent is from 1 to 3.5%; the mass percentage of the antioxidant is from 1.9 to 7%.
  • the inventors of the present application have found through repeated tests that when the additive includes a coupling agent, a stabilizer, a plasticizer and an antioxidant, the stability of the obtained MT ferrule raw material is significantly stronger than when only some of the additives are used. The obtained MT ferrule raw material.
  • the first high-speed stirring rate in the step (1) is 2000-5000r/min, the first time The ultrasonic power is 2000-8000W, and the first ultrasonic treatment time is 1 ⁇ 3h;
  • the second high-speed stirring rate in the step (1) is 3000-6000r/min, the second ultrasonic power is 2000-8000W, and the second ultrasonic processing time is 4-48h;
  • the drying temperature is 60 to 100 ° C, and the drying time is 1 to 10 days.
  • the filler microspheres prepared in the step (1) have a particle size of 0.5 to 70 um, wherein the filler microspheres have an average particle size of 6 to 15 um.
  • a method for preparing a MT ferrule raw material comprising the following steps:
  • the alumina microspheres treated with the coupling agent are premixed with PPS, and then melt blended by using a twin-screw extruder to prepare a composite material in which alumina microspheres are uniformly dispersed in a PPS resin matrix.
  • MT ferrule raw materials MT ferrule raw materials.
  • the polyphenylene sulfide is 35 parts by mass
  • the premixing stirring rate is 1000 r/min
  • the stirring temperature is ⁇ 80 °C.
  • Extrusion temperature of twin-screw extruder temperature in one zone: 260-280 °C; temperature in two zones: 290-310 °C; temperature in three zones: 300-320 °C; temperature in four zones: 300-320 °C; temperature in five zones: 300 ⁇ 320 ° C, screw speed 50r / min.
  • the MT ferrule raw material prepared in this embodiment has better dimensional stability than the SiO 2 composite material; the dimensional stability can be expressed by the thermal expansion coefficient, and the commercially available silica composite material has a thermal expansion coefficient of generally 13 ⁇ 17PPm/K, the strength is 80-120MPa, and the MT ferrule raw material obtained by the present embodiment has a thermal expansion coefficient of 12PPm/K and a strength of 144 MPa.
  • a method for preparing a MT ferrule raw material comprising the following steps:
  • the iron oxide and zinc oxide microspheres prepared by the coupling agent are prepared, wherein the stearic acid amide is 1.5 parts by mass, the high-speed stirring rate is 3800r/min, the ultrasonic power is 3500W, the processing time is 15h, and the drying is performed.
  • the temperature is 70 ° C and the drying time is 3 days; the prepared zirconium dioxide microspheres have a particle size of 0.5 to 90 ⁇ m, and the zirconium dioxide microspheres have an average particle size of 6 to 15 ⁇ m.
  • the iron oxide and zinc oxide microspheres treated by the coupling agent are premixed with PPS, and then melt blended by using a twin-screw extruder to prepare iron oxide and zinc oxide microspheres uniformly dispersed in the PPS resin matrix.
  • the composite material that is, the MT ferrule raw material.
  • Extrusion temperature of twin-screw extruder temperature in one zone: 260-280 °C; temperature in two zones: 290-310 °C; temperature in three zones: 300-320 °C; temperature in four zones: 300-320 °C; temperature in five zones: 300 ⁇ 320 ° C, screw speed 90r / min.
  • the MT ferrule raw material prepared in this embodiment has better dimensional stability than the SiO 2 composite material; the dimensional stability can be expressed by the thermal expansion coefficient, and the commercially available silica composite material has a thermal expansion coefficient of generally 13 ⁇ 17PPm/K, the strength is 80-120MPa, and the MT ferrule raw material obtained by the present embodiment has a thermal expansion coefficient of 13PPm/K and a strength of 130MPa.
  • a method for preparing a MT ferrule raw material comprising the following steps:
  • a coupling agent a mixture of ⁇ -glyceryloxypropyltrimethoxysilane and ⁇ -methacryloyloxytrimethoxysilane in a mass ratio of 3:1
  • the uniformly dispersed zirconia organic solution is subjected to high-speed stirring and ultrasonic treatment for a certain period of time, and then dried at a certain temperature for a certain period of time to obtain a zirconia microsphere after the coupling agent treatment, wherein ⁇ by mass - 2 parts mixture of glyceryloxypropyltrimethoxysilane and ⁇ -methacryloyloxytrimethoxysilane, high-speed stirring rate of 4400r/min, ultrasonic power of 5000W, treatment time of 26h, drying temperature
  • the drying time is 5 days at 80 ° C; the prepared zirconium dioxide microspheres have a particle size of 0.5-90 um, and the zirconium dioxide microspheres have an average particle size of 6
  • the ZrO 2 microspheres treated with the coupling agent are premixed with PPS, and then melt blended by a twin-screw extruder to prepare a composite material in which ZrO 2 microspheres are uniformly dispersed in the PPS resin matrix, thereby preparing the composite material.
  • MT ferrule raw materials are 27 parts by mass
  • the premixing stirring rate is 1500 r/min
  • the stirring temperature is ⁇ 80 °C.
  • Extrusion temperature of twin-screw extruder temperature in one zone: 260-280 °C; temperature in two zones: 290-310 °C; temperature in three zones: 300-320 °C; temperature in four zones: 300-320 °C; temperature in five zones: 300 ⁇ 320 ° C, screw speed 130r / min.
  • the MT ferrule raw material prepared in this embodiment has better dimensional stability than the SiO 2 composite material; the dimensional stability can be expressed by the thermal expansion coefficient, and the commercially available silica composite material has a thermal expansion coefficient of generally 13 -17PPm/K, the strength is 80-120MPa, and the MT ferrule raw material obtained by the present embodiment has a thermal expansion coefficient of 10PPm/K and a strength of 160MPa.
  • a method for preparing a MT ferrule raw material comprising the following steps:
  • the calcium carbonate microspheres after the coupling agent treatment were prepared, wherein 0.5 parts by mass of ⁇ -mercaptopropyltrimethoxysilane, a high-speed stirring rate of 5200 r/min, and an ultrasonic power of 6500 W, treatment time It is 37h, the drying temperature is 90 ° C, and the drying time is 7 days; the obtained calcium carbonate microspheres have a particle size of 0.5 to 90 um, and the calcium carbonate microspheres have an average particle size of 6 to 15 um.
  • the calcium carbonate microspheres treated by the coupling agent are premixed with PPS, and then melt blended by using a twin-screw extruder to prepare a composite material in which calcium carbonate microspheres are uniformly dispersed in a PPS resin matrix.
  • MT ferrule raw materials 21 parts by mass of polyphenylene sulfide, premixed stirring speed Rate: 1750r/min, stirring temperature ⁇ 80 °C.
  • Extrusion temperature of twin-screw extruder temperature in one zone: 260-280 °C; temperature in two zones: 290-310 °C; temperature in three zones: 300-320 °C; temperature in four zones: 300-320 °C; temperature in five zones: 300 ⁇ 320 ° C, screw speed 170r / min.
  • the MT ferrule raw material prepared in this embodiment has better dimensional stability than the SiO 2 composite material; the dimensional stability can be expressed by the thermal expansion coefficient, and the commercially available silica composite material has a thermal expansion coefficient of generally 13 ⁇ 17PPm/K, the strength is 80-120MPa, and the MT ferrule raw material obtained by the present embodiment has a thermal expansion coefficient of 12PPm/K and a strength of 139 MPa.
  • a method for preparing a MT ferrule raw material comprising the following steps:
  • the zirconia and alumina microspheres treated with the coupling agent are premixed with PPS, and then melt blended using a twin-screw extruder to prepare a zirconium dioxide and alumina microspheres uniformly dispersed in the PPS resin matrix.
  • the MT ferrule raw material is produced.
  • the polyphenylene sulfide is 14.5 parts by mass
  • the premixing stirring rate is 2000 r/min
  • the stirring temperature is ⁇ 80 °C.
  • Extrusion temperature of twin-screw extruder temperature in one zone: 260-280 °C; temperature in two zones: 290-310 °C; temperature in three zones: 300-320 °C; temperature in four zones: 300-320 °C; temperature in five zones: 300 ⁇ 320 ° C, screw speed 200r / min.
  • the MT ferrule raw material prepared in this embodiment has better dimensional stability than the SiO 2 composite material; the dimensional stability can be expressed by the thermal expansion coefficient, and the commercially available silica composite material has a thermal expansion coefficient of generally 13 ⁇ 17PPm/K, the strength is 80-120MPa, and the MT ferrule raw material obtained by the present embodiment has a thermal expansion coefficient of 11PPm/K and a strength of 152 MPa.
  • the MT ferrule is prepared by using the existing raw material SiO 2 , if the fluidity during molding is improved, the mechanical properties are lowered, and the size of the filler microspheres in the present invention is easy to control, the thermal stability is better, and the surface can be better. Modification, so that the filler particles are better combined with PPS, and the obtained ferrule material has better mechanical properties.
  • the ferrule raw material comprises the following components in terms of mass percentage: 14.5 polyphenylene sulfide, 14.4% tribasic lead sulfate, 0.1% 3-methyl acrylate Lipoxytrimethoxysilane and 71% iron oxide.
  • the MT ferrule raw material preparation method of the present embodiment is the same as that of the embodiment 2 except that the coupling agent and the stabilizer (tribasic lead sulfate) are added to the organic solution of the dispersed inorganic filler.
  • the ferrule raw material comprises the following components in terms of mass percentage: 17% polyphenylene sulfide, 0.1% di(2-ethylhexyl) phthalate, 13.5% 2,6-di-tert-butyl-4-methylphenol, 0.4% gamma-mercaptopropyltrimethoxysilane and 69% zinc oxide.
  • the preparation method of the MT ferrule raw material of the present embodiment is the same as that of the third embodiment except that the coupling agent is added to the organic solution of the dispersed inorganic filler, and the plasticizer (bis(2-ethyl) phthalate Ethyl ester) and antioxidant (2,6-di-tert-butyl-4-methylphenol).
  • the coupling agent is added to the organic solution of the dispersed inorganic filler, and the plasticizer (bis(2-ethyl) phthalate Ethyl ester) and antioxidant (2,6-di-tert-butyl-4-methylphenol).
  • the ferrule raw material comprises the following components in mass percentage: 21% polyphenylene sulfide, 0.17% bismuth laurate, 1% DINP and DNOP (wherein DINP and The mass ratio of DNOP is 1:4), 10.13% of antioxidant 1010, 0.7% of vinyl silane and stearic acid amide (wherein the mass ratio of vinyl silane to stearic acid amide is 1:1) and 67% Zirconium dioxide.
  • the preparation method of the MT ferrule raw material of the present embodiment is the same as that of the third embodiment except that the coupling agent is added to the organic solution of the dispersed inorganic filler, and the stabilizer (yttrium laurate) and the plasticizer (DINP and DNOP) and antioxidants (antioxidant 1010).
  • the ferrule raw material comprises the following components in mass percentage: 23.5% polyphenylene sulfide, 3% isooctyl dimethyl dimercaptoacetate, 4% Dilauryl thiodipropionate and triphenyl thiophosphite (mass ratio of dilauryl thiodipropionate and triphenyl thiophosphite 2:1), 3.5% DBP, 1% ⁇ -methacryloyloxytrimethoxysilane and 65% of zirconium dioxide and aluminum oxide (wherein the mass ratio of zirconium dioxide to aluminum oxide is 2:1).
  • the preparation method of the MT ferrule raw material of the present embodiment is the same as that of the embodiment 4 except that the coupling agent is added to the organic solution of the dispersed inorganic filler, and the stabilizer (isooctyl dimethyl dimercaptoacetate) is also added. , plasticizer (DBP) and antioxidants (dilauryl thiodipropionate and triphenyl thiophosphite).
  • the ferrule raw material comprises the following components in terms of mass percentage: 26% polyphenylene sulfide, 1.2% dibasic lead phosphite and lead stearate (dibasic The mass ratio of lead phosphite to lead stearate is 1:1), 3.5% DBP, DMP and DEP (mass ratio of DBP, DMP and DEP is 1:2:1), 7% of 2,6- Di-tert-butyl-4-methylphenol, 1.3% vinyl silane and 61% calcium carbonate.
  • the preparation method of the MT ferrule raw material of the present embodiment is the same as that of the embodiment 2 except that the coupling agent is added to the organic solution of the dispersed inorganic filler, and the stabilizer (dibasic lead phosphite and lead stearate) ), plasticizers (DBP, DMP and DEP) and antioxidants (2,6-di-tert-butyl-4-methylphenol).
  • the coupling agent is added to the organic solution of the dispersed inorganic filler, and the stabilizer (dibasic lead phosphite and lead stearate) ), plasticizers (DBP, DMP and DEP) and antioxidants (2,6-di-tert-butyl-4-methylphenol).
  • the ferrule raw material comprises the following components in mass percentage: 29.5% polyphenylene sulfide, 1.7% lead 2-ethyl acetate, 8.3% DMP, 1.9% Dilauryl thiodipropionate, 1.6% stearic acid amide and 57% zirconium dioxide.
  • the preparation method of the MT ferrule raw material of the present embodiment is the same as that of the third embodiment, except that the coupling agent is added to the organic solution of the dispersed inorganic filler, and the stabilizer (2-ethyl acetate lead) and the plasticizer are added. (DMP) and an antioxidant (dilauryl thiodipropionate).
  • the ferrule raw material comprises the following components in terms of mass percentage: 35% polyphenylene sulfide, 7.87% cadmium stearate, 0.13% antioxidant 1010, 2 % ⁇ -glyceryloxypropyltrimethoxysilane and 55% alumina.
  • the MT ferrule raw material preparation method of the present embodiment is the same as that of the embodiment 4 except that the coupling agent, the stabilizer (cadmium stearate) and the antioxidant (antioxidation) are added to the organic solution of the dispersed inorganic filler. Agent 1010).
  • Example 13 MT ferrule raw material stability test of the present invention
  • Test object MT ferrule raw materials prepared in Examples 2, 3, 4, 6, 7, 8, 9, 10, 11, and 12;
  • Test method detection by thermal expansion coefficient meter
  • Sample preparation diameter 3-5mm height 4-6mm; test temperature range: 0-150 ° C;
  • Heating rate 5 ° C / min
  • Example 10 MT ferrule raw material Thermal expansion coefficient (PPm/K) Example 2 13.4
  • Example 3 11.8
  • Example 4 12.4
  • Example 6 10.5
  • Example 7 11.2
  • Example 8 10.7
  • Example 9 10.1
  • Example 10 11.1
  • Example 11 10.8
  • Example 12 10.3
  • Example 14 Effect of inorganic fillers on mechanical properties of MT ferrule raw materials
  • Test object MT ferrule raw material, including the control group and the MT ferrule raw materials of Examples 4, 9 and 12, wherein the raw material ratio and preparation method of the control group were the same as those of Example 4 except that the inorganic filler was only used.
  • Test method test the impact strength by pendulum test
  • the impact strength of the MT ferrule raw material is significantly higher than that of other groups of MT ferrule raw materials, wherein the MT ferrule raw material when the inorganic filler is calcium carbonate The best impact strength.

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  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
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  • Organic Chemistry (AREA)
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  • Compositions Of Macromolecular Compounds (AREA)

Abstract

L'invention concerne une matière première de ferrule MT et un procédé de préparation associé. Ladite matière première de ferrule comprend les composants suivants en pourcentage en masse : 14,5 % à 35 % de sulfure de polyphénylène, et 55 % à 85 % d'une charge inorganique, la charge inorganique étant au moins l'un du dioxyde de zirconium, du dioxyde de silicium, de l'alumine, de l'oxyde de fer, de l'oxyde de zinc et du carbonate de calcium. Concernant les défauts de matières premières de ferrule MT existantes, la matière première de ferrule MT préparée par le procédé de la présente invention présente une meilleure stabilité dimensionnelle et un coefficient de dilatation thermique inférieur, tout en présentant des coûts inférieurs, et une durée de vie plus longue.
PCT/CN2017/093166 2017-01-26 2017-07-17 Matière première de ferrule mt et procédé de préparation associé WO2018137320A1 (fr)

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CN106832930A (zh) * 2017-01-26 2017-06-13 潮州三环（集团）股份有限公司 Mt插芯原材料及其制备方法
CN107674382B (zh) * 2017-09-28 2020-08-11 泰安盛源粉体有限公司 一种优化电工填料氧化铝粒度组成的方法
CN113316320A (zh) * 2021-04-13 2021-08-27 青岛中青电子软件有限公司 一种高导热pcb基板的加工制备方法

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