CN102732016A - Preparation method for silicon carbide reinforced nylon composite - Google Patents

Preparation method for silicon carbide reinforced nylon composite Download PDF

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Publication number
CN102732016A
CN102732016A CN2012101980027A CN201210198002A CN102732016A CN 102732016 A CN102732016 A CN 102732016A CN 2012101980027 A CN2012101980027 A CN 2012101980027A CN 201210198002 A CN201210198002 A CN 201210198002A CN 102732016 A CN102732016 A CN 102732016A
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CN
China
Prior art keywords
preparation
parts
silit
district
temperature
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN2012101980027A
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Chinese (zh)
Inventor
陶渭清
沈兴元
颜卫峰
陶立强
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SUZHOU YUDU MEDICAL INSTRUMENT CO Ltd
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SUZHOU YUDU MEDICAL INSTRUMENT CO Ltd
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Application filed by SUZHOU YUDU MEDICAL INSTRUMENT CO Ltd filed Critical SUZHOU YUDU MEDICAL INSTRUMENT CO Ltd
Priority to CN2012101980027A priority Critical patent/CN102732016A/en
Publication of CN102732016A publication Critical patent/CN102732016A/en
Pending legal-status Critical Current

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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/04Particle-shaped
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/36Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/395Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
    • B29C48/40Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/78Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling
    • B29C48/875Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling for achieving a non-uniform temperature distribution, e.g. using barrels having both cooling and heating zones
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/92Measuring, controlling or regulating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00Indexing scheme relating to extrusion moulding
    • B29C2948/92Measuring, controlling or regulating
    • B29C2948/92504Controlled parameter
    • B29C2948/92704Temperature
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00Indexing scheme relating to extrusion moulding
    • B29C2948/92Measuring, controlling or regulating
    • B29C2948/92819Location or phase of control
    • B29C2948/92857Extrusion unit
    • B29C2948/92876Feeding, melting, plasticising or pumping zones, e.g. the melt itself
    • B29C2948/92895Barrel or housing

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention provides a preparation method for a silicon carbide reinforced nylon composite, which belongs to the technical field of preparation of high-molecular materials. The method comprises the following steps: weighing 70 to 80 parts by weight of nylon 66 resin, 30 to 36 parts by weight of nylon 6 resin, 0.9 to 1.5 parts by weight of a coupling agent, 19 to 27 parts by weight of a filling material and 5 to 11 parts by weight of silicon carbide, fully mixing the above-mentioned components in a mixer with mixing time being 12 to 18 min and the rotating speed of the mixer being 600 to 1000 n/min, then adding 0.5 to 0.9 part by weight of an anti-oxidant, 30 to 41 parts by weight of glass fibers and 0.3 to 0.7 part by weight of a surface modifier and continuing full mixing for 2 to 6 min so as to obtain a granulated material; and adding the granulated material into a double-screw extruder for melt extrusion and respectively setting temperature of each heating zone of screws so as to obtain the silicon carbide reinforced nylon composite. The preparation method provided in the invention has the following advantages: process steps are simple and concise; and the prepared composite has excellent mechanical properties and is applicable to preparation of demanding parts used in the fields of military matters, spaceflight, automobiles, buildings and the like.

Description

The preparation method of silit enhanced nylon composite materials
Technical field
The invention belongs to field of polymer material preparing technology, be specifically related to a kind of preparation method of silit enhanced nylon composite materials
Background technology
silit is a kind of good atomic crystal material, and its carbon and silicon combine by the covalency bonding force.Therefore, silit has excellent mechanical property, thermotolerance, erosion resistance, is mainly used in space flight and military field.In recent years, because technical progress, the production cost of silit constantly reduces, thereby this material is able to from the high-end field to extending such as fields such as automobile, buildings.Reflect this, the preparation method of the nylon composite materials that exploration silit increases has good realistic meaning, and the technical scheme that will introduce below produces under this background
Summary of the invention
task of the present invention is to provide a kind of preparation method of silit enhanced nylon composite materials; This method technology is terse and can satisfy the industrial amplification production requirement; And the material that obtains has excellent mechanical property, is suitable for the product that fields such as military affairs, space flight, automobile, building make high request.
Task of the present invention is accomplished like this, and a kind of preparation method of silit enhanced nylon composite materials may further comprise the steps:
A) preparation granulation material; Thorough mixing in 70~80 parts of the Nylon 66s that will take by weighing by weight earlier, 30~36 parts of Nylon 6s, 0.9~1.5 part of coupling agent, 19~27 parts of fillers and 5~11 parts of input mixing machines of silit; Mixing time is 12-18min; The rotating speed of mixing machine is 600-1000n/min, drops into 0.3~0.7 part of 30~41 parts in 0.5~0.9 part in oxidation inhibitor, spun glass that parts by weight take by weighing and surface-modifying agent again, continues thorough mixing; Mixing time is 2-6min, obtains the granulation material;
B) granulation, with melt extruding in the granulation material input twin screw extruder, wherein: each heating region temperature setting of screw rod is respectively: 230 ℃ of district's temperature; 235 ℃ of two district's temperature, 235 ℃ of three district's temperature, 240 ℃ of four district's temperature; 240 ℃ of five district's temperature, 245 ℃ of six district's temperature, 245 ℃ of seven district's temperature; 250 ℃ of eight district's temperature, 250 ℃ of nine district's temperature obtain silit enhanced nylon composite materials.
in one embodiment of the invention, described Nylon 66 is a fusing point at 240 ℃ resin.
in another embodiment of the present invention, described Nylon 6 is a fusing point at 210 ℃ resin.
in yet another embodiment of the present invention, described coupling agent is β-(3,4 epoxy cyclohexyl) ethyl trimethoxy silane.
in another embodiment of the present invention, described filler is surface treated white mica.
also have among the embodiment of the present invention, and described silit is that length-to-diameter ratio is 80~120 silicon carbide fiber.
are more of the present invention and among embodiment, described oxidation inhibitor is two (2,4 di-tert-butyl-phenyl) pentaerythritol diphosphites.
in of the present invention and then embodiment, described spun glass is the alkali-free short glass fiber of length 3mm.
of the present invention again more and among embodiment, described surface-modifying agent is an amine hydroxybenzene.
Technical scheme process step provided by the invention is very terse and help suitability for industrialized production, and the tensile strength of the material that obtains is greater than 155MPa, and flexural strength is greater than 253MPa, and the socle girder notched Izod impact strength is greater than 27 .5kj/m 2 , melting index is greater than 17g/10min, because superior and the parts of high request are made in fields such as applicable military affairs, space flight, automobile and building.
Embodiment
Embodiment 1:
A) preparation granulation material; The fusing point that will take by weighing by weight earlier is that 240 ℃ resin is that 70 parts of Nylon 66s, fusing point are that 36 parts of Nylon 6s, coupling agent are β-(3 at 210 ℃ resin; 4 epoxy cyclohexyls) 1.2 parts of ethyl trimethoxy silanes, filler are that 19 parts of surface treated white micas and length-to-diameter ratio are that 80~120 silicon carbide fiber is put into for 5 parts and mixed 18min in the mixing machine; The rotating speed of mixing machine is 600n/min; Dropping into the oxidation inhibitor that takes by weighing by weight again is two (2; 4 di-tert-butyl-phenyls) 32 parts of the alkali-free short glass fibers of 0.7 part of pentaerythritol diphosphites, length 3mm and surface-modifying agent are 0.3 part of amine hydroxybenzene, continue to mix 2min, obtain the granulation material;
B) granulation will be by steps A) the granulation material that obtains drops in the twin screw extruder and melt extrudes, and wherein: each heating region temperature setting of screw rod is respectively: 230 ℃ of district's temperature; 235 ℃ of two district's temperature, 235 ℃ of three district's temperature, 240 ℃ of four district's temperature; 240 ℃ of five district's temperature, 245 ℃ of six district's temperature, 245 ℃ of seven district's temperature; 250 ℃ of eight district's temperature, 250 ℃ of nine district's temperature obtain silit enhanced nylon composite materials.
Embodiment 2:
A) preparation granulation material; The fusing point that will take by weighing by weight earlier is that 240 ℃ resin is that 72 parts of Nylon 66s, fusing point are that 30 parts of Nylon 6s, coupling agent are β-(3 at 210 ℃ resin; 4 epoxy cyclohexyls) 0.9 part of ethyl trimethoxy silane, filler are that 27 parts of surface treated white micas and length-to-diameter ratio are that 80~120 silicon carbide fiber is put into for 7 parts and mixed 13min in the mixing machine; The rotating speed of mixing machine is 1000n/min; Dropping into the oxidation inhibitor that takes by weighing by weight again is two (2; 4 di-tert-butyl-phenyls) 33 parts of the alkali-free short glass fibers of 0.4 part of pentaerythritol diphosphites, length 3mm and surface-modifying agent are 0.3 part of amine hydroxybenzene, continue to mix 3min, obtain the granulation material.All the other are all with the description to embodiment 1.
Embodiment 3:
A) preparation granulation material; The fusing point that will take by weighing by weight earlier is that 240 ℃ resin is that 80 parts of Nylon 66s, fusing point are that 34 parts of Nylon 6s, coupling agent are β-(3 at 210 ℃ resin; 4 epoxy cyclohexyls) 1.5 parts of ethyl trimethoxy silanes, filler are that 24 parts of surface treated white micas and length-to-diameter ratio are that 80~120 silicon carbide fiber is put into for 11 parts and mixed 14min in the mixing machine; The rotating speed of mixing machine is 800n/min; Dropping into the oxidation inhibitor that takes by weighing by weight again is two (2; 4 di-tert-butyl-phenyls) 41 parts of the alkali-free short glass fibers of 0.9 part of pentaerythritol diphosphites, length 3mm and surface-modifying agent are 0.7 part of amine hydroxybenzene, continue to mix 4min, obtain the granulation material.All the other are all with the description to embodiment 1.
Embodiment 4:
A) preparation granulation material; The fusing point that will take by weighing by weight earlier is that 240 ℃ resin is that 76 parts of Nylon 66s, fusing point are that 32 parts of Nylon 6s, coupling agent are β-(3 at 210 ℃ resin; 4 epoxy cyclohexyls) 1.3 parts of ethyl trimethoxy silanes, filler are that 21 parts of surface treated white micas and length-to-diameter ratio are that 80~120 silicon carbide fiber is put into for 9 parts and mixed 16min in the mixing machine; The rotating speed of mixing machine is 700n/min; Dropping into the oxidation inhibitor that takes by weighing by weight again is two (2; 4 di-tert-butyl-phenyls) 37 parts of the alkali-free short glass fibers of 0.8 part of pentaerythritol diphosphites, length 3mm and surface-modifying agent are 0.5 part of amine hydroxybenzene, continue to mix 6min, obtain the granulation material.All the other are all with the description to embodiment 1.
The silit enhanced nylon composite materials that is obtained by the foregoing description 1-4 has the technique effect shown in the following table through test:
Test event Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4
Tensile strength MPa 155 158 161 164
Flexural strength MPa 253 257 261 265
Socle girder notched Izod impact strength kj/m 2 27.5 27.8 28.2 28.6
Melting index g/10min 17 17.4 17.8 18.2

Claims (9)

1. A kind of preparation method of silit enhanced nylon composite materials is characterized in that may further comprise the steps:
A) preparation granulation material; Thorough mixing in 70~80 parts of the Nylon 66s that will take by weighing by weight earlier, 30~36 parts of Nylon 6s, 0.9~1.5 part of coupling agent, 19~27 parts of fillers and 5~11 parts of input mixing machines of silit; Mixing time is 12-18min; The rotating speed of mixing machine is 600-1000n/min, drops into 0.3~0.7 part of 30~41 parts in 0.5~0.9 part in oxidation inhibitor, spun glass that parts by weight take by weighing and surface-modifying agent again, continues thorough mixing; Mixing time is 2-6min, obtains the granulation material;
B) granulation, with melt extruding in the granulation material input twin screw extruder, wherein: each heating region temperature setting of screw rod is respectively: 230 ℃ of district's temperature; 235 ℃ of two district's temperature, 235 ℃ of three district's temperature, 240 ℃ of four district's temperature; 240 ℃ of five district's temperature, 245 ℃ of six district's temperature, 245 ℃ of seven district's temperature; 250 ℃ of eight district's temperature, 250 ℃ of nine district's temperature obtain silit enhanced nylon composite materials.
2. the preparation method of silit enhanced nylon composite materials according to claim 1 is characterized in that described Nylon 66 is a fusing point at 240 ℃ resin.
3. the preparation method of silit enhanced nylon composite materials according to claim 1 is characterized in that described Nylon 6 is a fusing point at 210 ℃ resin.
4. the preparation method of silit enhanced nylon composite materials according to claim 1 is characterized in that described coupling agent is β-(3,4 epoxy cyclohexyl) ethyl trimethoxy silane.
5. the preparation method of silit enhanced nylon composite materials according to claim 1 is characterized in that described filler is surface treated white mica.
6. the preparation method of silit enhanced nylon composite materials according to claim 1 is characterized in that described silit is that length-to-diameter ratio is 80~120 silicon carbide fiber.
7. the preparation method of silit enhanced nylon composite materials according to claim 1 is characterized in that described oxidation inhibitor is two (2,4 di-tert-butyl-phenyl) pentaerythritol diphosphites.
8. the preparation method of silit enhanced nylon composite materials according to claim 1 is characterized in that described spun glass is the alkali-free short glass fiber of length 3mm.
9. The preparation method of silit enhanced nylon composite materials according to claim 1 is characterized in that described surface-modifying agent is an amine hydroxybenzene
CN2012101980027A 2012-06-15 2012-06-15 Preparation method for silicon carbide reinforced nylon composite Pending CN102732016A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104387767A (en) * 2014-12-17 2015-03-04 天津金发新材料有限公司 Ceramic fiber reinforced nylon 66(PA66) composite and preparation method thereof
CN104910618A (en) * 2015-05-29 2015-09-16 苏州博利迈新材料科技有限公司 Anti-static and halogen-free flame-retardant PA66 composition and preparation method thereof
CN110305472A (en) * 2019-07-26 2019-10-08 泉州志山阀门有限公司 A kind of nylon valve body material and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102108204A (en) * 2009-12-24 2011-06-29 合肥杰事杰新材料有限公司 Plastic case material for breaker and preparation method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102108204A (en) * 2009-12-24 2011-06-29 合肥杰事杰新材料有限公司 Plastic case material for breaker and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104387767A (en) * 2014-12-17 2015-03-04 天津金发新材料有限公司 Ceramic fiber reinforced nylon 66(PA66) composite and preparation method thereof
CN104910618A (en) * 2015-05-29 2015-09-16 苏州博利迈新材料科技有限公司 Anti-static and halogen-free flame-retardant PA66 composition and preparation method thereof
CN110305472A (en) * 2019-07-26 2019-10-08 泉州志山阀门有限公司 A kind of nylon valve body material and preparation method thereof

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Application publication date: 20121017