CN103772922A - Antiflaming, insulative and heat conductive polybutylene terephthalate composite material and preparation method thereof - Google Patents
Antiflaming, insulative and heat conductive polybutylene terephthalate composite material and preparation method thereof Download PDFInfo
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- CN103772922A CN103772922A CN201210414484.5A CN201210414484A CN103772922A CN 103772922 A CN103772922 A CN 103772922A CN 201210414484 A CN201210414484 A CN 201210414484A CN 103772922 A CN103772922 A CN 103772922A
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- 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
- B29C48/03—Extrusion 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
- B29C48/04—Particle-shaped
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- 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
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/395—Means 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
- B29C48/40—Means 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
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- 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
- B29C48/78—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling
- B29C48/875—Thermal 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
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- 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
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- 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
- B29C2948/92695—Viscosity; Melt flow index [MFI]; Molecular weight
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- 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
-
- 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
- B29C2948/92819—Location or phase of control
- B29C2948/92857—Extrusion unit
- B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
- B29C2948/92895—Barrel or housing
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- 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
- B29C2948/92819—Location or phase of control
- B29C2948/92923—Calibration, after-treatment or cooling zone
Abstract
The invention relates to an antiflaming, insulative and heat conductive polybutylene terephthalate composite material and a preparation method thereof. The composite material comprises the following components in parts by weight: 25 to 37 parts of PBT, 55 to 67 parts of a heat conductive filling material, 0.3 to 0.4 part of an anti-oxidant, 0.5 to 0.7 part of a coupling agent, 0.5 to 0.7 part of a liquid addition agent, 2.0 to 5.0 parts of a toughening agent, 0.5 to 0.7 part of a lubricating agent, 3.0 to 6.0 parts of a flame retardant and 1.0 to 2.0 parts of a flame retardant synergist. The preparation method for the composite material comprises the following steps: (1)mixing the coupling agent and the liquid addition agent, adding into the dried heat conductive filling material, stirring in a high-mixing machine for 30 min, and drying at 100 DEG C for 3 hours for standby; (2)putting the dried PBT, the anti-oxidant, the lubricating agent, the toughening agent, the flame retardant, the flame retardant synergist and the material obtained in the step (1) into a high speed mixer, stirring for 15 min, putting into an extruding machine, and performing extrusion granulation. Compared with the prior art, high-fluidity matrix resin, the cheap heat conductive filling material and the efficient environment-friendly brominated flame retardant are adopted, the cost of the composite material is enabled to be reduced, and higher heat conductivity and good flame retardant property are achieved.
Description
Technical field
The invention belongs to field of functional polymer composites, especially relate to a kind of fire retardant insulating heat conduction polybutylene terephthalate matrix material and preparation method.
Background technology
Polybutylene terephthalate (PBT) thermoplastic engineering plastic is one of five large general engineering plastic, is industrialization kind with fastest developing speed still the latest in general engineering plastic.PBT has high heat resistance, and life-time service temperature (RTI) can reach 140 ℃; Low water absorption is only 1%; Still can keep in a humid environment various physical property, comprise electrical insulating property; In addition, PBT also has resistance to fatigue, weathering resistance, chemical proofing, good fluidity, and easily machine-shaping and shaping cycle are short, and product surface is smooth, glossiness is high.The over-all properties that it is excellent and processing characteristics are widely used in the industries such as electronic apparatus, automobile, light fixture it.Along with scientific and technical development, the miniaturization of microelectronic Highgrade integration, device, hope extends the life-span of device, requires PBT also to need to have higher heat conductivility, so that the heat radiation of system, device.PBT is a kind of polymer organic polymer (degree of crystallinity 40%), thermal conductivity is about 0.22w/mK, can not meet radiating requirements, therefore, people as graphite, carbon fiber, metal-powder, aluminium nitride, boron nitride, aluminum oxide, silicon carbide etc. carry out the compound PBT heat-conducting plastic that obtains with PBT, have increased substantially the heat conductivility of PBT by filler high thermal conductivity.But a lot of electronic enterprises, as shells such as LED, need heat conductive flame-retarding material, this just need to carry out flame-retardant modified to heat conduction PBT.About heat conductive flame-retarding PBT, Chinese patent CN200810198652.5 assembles phosphorus flame retardant and heat conductive filler magnesium oxide to obtain heat conductive flame-retarding agent, and magnesium oxide is to the heat conductivility raising effect of system little; Patent CN201010194959.5 discloses the material of a kind of aluminium nitride filling PBT, but this material does not reach the fire-retardant requirement of V-0 level; Patent CN200910055634.6 discloses a kind of enhancing flame-retarded heat-conducting PBT material, fills PBT material but this patent only discloses nano aluminum nitride, and the processing of nano material is cumbersome and price is also higher.
Summary of the invention
Object of the present invention is exactly to provide a kind of fire retardant insulating heat conduction polybutylene terephthalate matrix material and preparation method in order to overcome the defect that above-mentioned prior art exists.
Object of the present invention can be achieved through the following technical solutions:
A kind of fire retardant insulating heat conduction polybutylene terephthalate matrix material, this matrix material is made up of the component that comprises following weight part:
Described PBT is middle low viscosity kind, and melting index is greater than 50g/10min (250 ℃, 2.16Kg); Described heat conductive filler is selected from one or more in silicon carbide, aluminum oxide, boron nitride or aluminium nitride; Described oxidation inhibitor is the composite of Hinered phenols primary antioxidant and phosphorous acid esters auxiliary antioxidant.
A kind of in the preferred silicon carbide of described heat conductive filler or aluminum oxide or both is composite.
Described Hinered phenols primary antioxidant is N; N '-bis--(3-(3; 5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine (oxidation inhibitor 1098); described phosphorous acid esters auxiliary antioxidant is three [2.4-di-tert-butyl-phenyl] phosphorous acid esters (irgasfos 168) or 4; 4 '-[1; 1 '-xenyl] subunit di 2 ethylhexyl phosphonic acid-tetra-[2,4-, bis-trimethylphenylmethane bases] ester (oxidation inhibitor PEPQ).
Described coupling agent is selected from titante coupling agent or silane coupling agent; Described liquid adjuvants is commercially available white oil; Described toughner is ethylene-methyl acrylate-glyceryl methacrylate terpolymer; Described lubricant is selected from silicone or pentaerythritol stearate (PETs); Described fire retardant is environmental protection bromide fire retardant, is selected from TDE or brominated styrene; Described fire retarding synergist is antimonous oxide.
Preferred γ-the glycidyl ether oxygen propyl trimethoxy silicane of described coupling agent (KH550).
The preferred TDE of described fire retardant.
A preparation method for fire retardant insulating heat conduction polybutylene terephthalate matrix material, the method comprises the following steps:
(1) after 0.5～0.7 part of coupling agent is mixed with 0.5～0.7 part of liquid adjuvants, join in 55～67 parts of dry heat conductive fillers, in high mixer, stir 30 minutes, for subsequent use after dry 3h at 100 ℃;
(2) by 25～37 parts of dry PBT, 0.3～0.4 part of oxidation inhibitor, 0.5～0.7 part of lubricant, 2.0～5.0 parts of toughner, 3.0～6.0 parts of fire retardants, 1.0～2.0 parts of fire retarding synergists and step (1) gains, put into high-speed mixer, stir after 15 minutes, put into forcing machine extruding pelletization.
The mode that coupling agent in step (1) and liquid adjuvants join in heat conductive filler adds for spraying; In step (1), dry heat conductive filler refers to the heat conductive filler after dry 4h at 80 ℃; In step (2), dry PBT refers to the PBT after dry 4h at 100 ℃.
Described forcing machine is the twin screw extruder of six sections of heating, and the temperature in 1 district～6 district is respectively: 170～190 ℃, and 210～230 ℃, 230～250 ℃, 240～260 ℃, 240～260 ℃, 240～260 ℃, the head temperature of twin screw extruder is 230～250 ℃.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) the present invention adopts the matrix resin of high workability, and system workability is good, and mechanical property declines few.
(2) the present invention adopts cheap heat conductive filler, or cheap filler and high price filler composite, make material cost reduce.
(3) the present invention adopts high-efficiency environment friendly bromide fire retardant, and little on the loading level impact of heat conductive filler, material can have the flame retardant properties that higher thermal conductivity is become reconciled simultaneously.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
A kind of PBT thermally conductive material, mark by weight, is made up of following component:
(1) by 37 parts of PBT dry 4h at 100 ℃, by 55 parts of heat conduction silicon carbide dry 4h at 80 ℃;
(2) 55 parts of dried heat conduction silicon carbide are put into high mixer, mode by the mixture of 0.5 part of coupling agent KH550 and 0.5 part of white oil to spray, join in 55 parts of heat conduction silicon carbide in high-speed mixer, high-speed mixing 30 minutes, stand-by after dry 3h at 100 ℃;
(3) mixture 37 parts of dried PBT, 1098,0.25 part of irgasfos 168 of 0.15 part of oxidation inhibitor, 0.5 part of PETs, 2.0 parts of toughner ethylene-methyl acrylate-glyceryl methacrylate terpolymers (LOTADER AX8900), 6.0 parts of TDE, 2.0 parts of antimonous oxides and step 2 being obtained, put in high-speed mixer, at room temperature mix 15 minutes;
(4) compound of step (3) gained is joined in twin screw extruder, screw rod 1～6 district's temperature is respectively 180～200 ℃, 210～230 ℃, 220～240 ℃, 230～240 ℃, 220～240 ℃, 230～240 ℃, head is 230～240 ℃; Extruding pelletization.At 100 ℃, the particle that obtains, after dry 3h, be injection molded into exemplar, standby survey, the temperature of injection moulding machine is 230～280 ℃.
Sample mechanical property is by following standard testing, and result is as shown in table 1: this matrix material not only has higher thermal conductivity, also has higher heat-drawn wire and good mechanical property.
Table 1
| Performance | Embodiment 1 | Inspecting standard |
| Density (g/cm 3) | 2.02 | ISO1183 |
| Tensile strength (Mpa) | 72 | ISO 527-1 |
| Flexural strength (Mpa) | 125 | ISO 178 |
| Charpy notched Izod impact strength (KJ/m 2) | 6 | ISO179-1 |
| Flame retardant properties (1.6mm) | V-0 | UL 94 |
| In thermal conductivity (W/mK) layer | 1.1 | ASTME 1461-01 |
Embodiment 2
A kind of PBT thermally conductive material, mark by weight, is made up of following component:
(1) by 25 parts of PBT resins dry 4h at 100 ℃, by 67 parts of heat conduction aluminum oxide dry 4h at 80 ℃;
(2) 67 parts of dried heat conduction aluminum oxide are put into high mixer, by the mixture of 0.7 part of coupling agent and 0.7 part of white oil, join in 67 parts of heat conduction aluminum oxide in high-speed mixer in the mode of spraying, high-speed mixing is after 30 minutes, stand-by after dry 3h at 100 ℃;
(3) mixture 25 parts of dried PBT, 1098,0.2 part of PEPQ of 0.1 part of oxidation inhibitor, 0.7 part of silicone, 5.0 parts of toughner ethylene-methyl acrylate-glyceryl methacrylate terpolymers (LOTADER AX8900), 3.0 parts of TDE, 1.0 parts of antimonous oxides and step 2 being obtained, put in high-speed mixer, at room temperature mix 15 minutes;
(4) compound of step (3) gained is joined in twin screw extruder, screw rod 1～6 district's temperature is respectively 180～200 ℃, 210～230 ℃, 220～240 ℃, 230～240 ℃, 220～240 ℃, 230～240 ℃, head is 230～240 ℃; Extruding pelletization.At 100 ℃, the particle that obtains, after dry 3h, be injection molded into exemplar, standby survey, the temperature of injection moulding machine is 230～280 ℃.
Sample mechanical property is by following standard testing, and result is as shown in table 2: this matrix material not only has higher thermal conductivity, also has higher heat-drawn wire and good mechanical property.
Table 2
| Performance | Embodiment 2 | Inspecting standard |
| Density (g/cm 3) | 2.38 | ISO1183 |
| Tensile strength (Mpa) | 55 | ISO 527-1 |
| Flexural strength (Mpa) | 100 | ISO 178 |
| Charpy notched Izod impact strength (KJ/m 2) | 3 | ISO179-1 |
| Flame retardant properties (1.6mm) | V-0 | UL94 |
| Thermal conductivity (W/mK) | 1.0 | ASTME 1461-01 |
Embodiment 3
A kind of PBT thermally conductive material, mark by weight, is made up of following component:
(1) by 30 parts of PBT resins dry 4h at 100 ℃, by 62 parts of heat conduction aluminium nitride dry 4h at 80 ℃;
(2) 62 parts of dried heat conduction aluminium nitride are put into high mixer, by the mixture of 0.6 part of coupling agent and 0.6 part of white oil, in the mode of spraying, join 62 parts of heat conduction aluminium nitride in high-speed mixer, after high-speed mixing 30 minutes, stand-by after dry 3h at 100 ℃;
(3) mixture 30 parts of dried PBT, 1098,0.25 part of PEPQ of 0.1 part of oxidation inhibitor, 0.6 part of silicone, 4.0 parts of toughner ethylene-methyl acrylate-glyceryl methacrylate terpolymers (LOTADER AX8900), 4.5 parts of TDE, 1.5 parts of antimonous oxides and step 2 being obtained, put in high-speed mixer, at room temperature mix 15 minutes;
(4) compound of step (3) gained is joined in twin screw extruder, screw rod 1～6 district's temperature is respectively 180～200 ℃, 210～230 ℃, 220～240 ℃, 230～240 ℃, 220～240 ℃, 230～240 ℃, head is 230～240 ℃; Extruding pelletization.At 100 ℃, the particle that obtains, after dry 3h, be injection molded into exemplar, standby survey, the temperature of injection moulding machine is 230～280 ℃.
Sample mechanical property is by following standard testing, and result is as shown in table 3: this matrix material not only has higher thermal conductivity, also has higher heat-drawn wire and good mechanical property.
Table 3
| Performance | Embodiment 3 | Inspecting standard |
| Density (g/cm 3) | 2.08 | ISO1183 |
| Tensile strength (Mpa) | 60 | ISO 527-1 |
| Flexural strength (Mpa) | 110 | ISO 178 |
| Charpy notched Izod impact strength (KJ/m 2) | 4 | ISO179-1 |
| Flame retardant properties (1.6mm) | V-0 | UL94 |
| In thermal conductivity (W/mK) layer | 1.7 | ASTME 1461-01 |
Embodiment 4
A kind of PBT thermally conductive material, mark by weight, is made up of following component:
(1) by 35 parts of PBT dry 4h at 100 ℃, by 57 parts of heat conduction boron nitride dry 4h at 80 ℃;
(2) 57 parts of dried heat conduction boron nitride are put into high mixer, by the mixture of 0.6 part of coupling agent and 0.6 part of white oil, in the mode of spraying, join 57 parts of heat conduction boron nitride in high-speed mixer, after high-speed mixing 30 minutes, stand-by after dry 3h at 100 ℃;
(3) by 35 parts of dried PBT, the mixture that 1098,0.25 part of PEPQ of 0.15 part of oxidation inhibitor, 0.6 part of silicone, 3.0 parts of toughner ethylene-methyl acrylate-glyceryl methacrylate terpolymers (LOTADER AX8900), 6.0 parts of TDE, 2.0 parts of antimonous oxides and step 2 obtain, put in high-speed mixer, at room temperature mix 15 minutes;
(4) compound of step (3) gained is joined in twin screw extruder, screw rod 1～6 district's temperature is respectively 180～200 ℃, 210～230 ℃, 220～240 ℃, 230～240 ℃, 220～240 ℃, 230～240 ℃, head is 230～240 ℃; Extruding pelletization.At 100 ℃, the particle that obtains, after dry 3h, be injection molded into exemplar, standby survey, the temperature of injection moulding machine is 230～280 ℃.
Sample mechanical property is by following standard testing, and result is as shown in table 4: this matrix material not only has higher thermal conductivity, also has higher heat-drawn wire and good mechanical property.
Table 4
| Performance | Embodiment 4 | Inspecting standard |
| Density (g/cm 3) | 1.77 | ISO1183 |
| Tensile strength (Mpa) | 63 | ISO 527-1 |
| Flexural strength (Mpa) | 115 | ISO 178 |
| Charpy notched Izod impact strength (KJ/m 2) | 4 | ISO179-1 |
| Flame retardant properties (1.6mm) | V-0 | UL94 |
| In thermal conductivity (W/mK) layer | 2.1 | ASTME 1461-01 |
Embodiment 5
A kind of PBT thermally conductive material, mark by weight, is made up of following component:
(1) by 37 parts of PBT dry 4h at 100 ℃, by 35 parts of heat conduction silicon carbide and 20 parts of heat conduction aluminium nitride dry 4h at 80 ℃;
(2) dried 35 parts of heat conduction silicon carbide and 20 parts of heat conduction aluminium nitride are put into high mixer, mode by the mixture of 0.5 part of coupling agent KH550 and 0.5 part of white oil to spray, join in the 35 parts of heat conduction silicon carbide and 20 parts of heat conduction aluminium nitride in high-speed mixer, high-speed mixing 30 minutes, stand-by after dry 3h at 100 ℃;
(3) mixture 37 parts of dried PBT, 1098,0.25 part of irgasfos 168 of 0.15 part of oxidation inhibitor, 0.5 part of PETs, 2.0 parts of toughner ethylene-methyl acrylate-glyceryl methacrylate terpolymers (LOTADER AX8900), 6.0 parts of TDE, 2.0 parts of antimonous oxides and step 2 being obtained, put in high-speed mixer, at room temperature mix 15 minutes;
(4) compound of step (3) gained is joined in twin screw extruder, screw rod 1～6 district's temperature is respectively 180～200 ℃, 210～230 ℃, 220～240 ℃, 230～240 ℃, 220～240 ℃, 230～240 ℃, head is 230～240 ℃; Extruding pelletization.At 100 ℃, the particle that obtains, after dry 3h, be injection molded into exemplar, standby survey, the temperature of injection moulding machine is 230～280 ℃.
Sample mechanical property is by following standard testing, and result is as shown in table 5: this matrix material not only has higher thermal conductivity, also has higher heat-drawn wire and good mechanical property.
Table 5
| Performance | Embodiment 3 | Inspecting standard |
| Density (g/cm 3) | 2.02 | ISO1183 |
| Tensile strength (Mpa) | 69 | ISO 527-1 |
| Flexural strength (Mpa) | 120 | ISO 178 |
| Charpy notched Izod impact strength (KJ/m 2) | 5 | ISO179-1 |
| Flame retardant properties (1.6mm) | V-0 | UL94 |
| Thermal conductivity (W/mK) | 1.4 | ASTME 1461-01 |
Embodiment 6
A kind of PBT thermally conductive material, mark by weight, is made up of following component:
(1) by 37 parts of PBT dry 4h at 100 ℃, by 40 parts of heat conduction aluminum oxide and 15 parts of heat conduction aluminium nitride dry 4h at 80 ℃;
(2) dried 40 parts of heat conduction aluminum oxide and 15 parts of heat conduction boron nitride are put into high mixer, mode by the mixture of 0.5 part of coupling agent KH550 and 0.5 part of white oil to spray, join in the 340 parts of heat conduction aluminum oxide and 15 parts of heat conduction boron nitride in high-speed mixer, high-speed mixing 30 minutes, stand-by after dry 3h at 100 ℃;
(3) mixture 37 parts of dried PBT, 1098,0.25 part of oxidation inhibitor PEPQ of 0.15 part of oxidation inhibitor, 0.5 part of PETs, 2.0 parts of toughner ethylene-methyl acrylate-glyceryl methacrylate terpolymers (LOTADER AX8900), 6.0 parts of TDE, 2.0 parts of antimonous oxides and step 2 being obtained, put in high-speed mixer, at room temperature mix 15 minutes;
(4) compound of step (3) gained is joined in twin screw extruder, screw rod 1～6 district's temperature is respectively 180～200 ℃, 210～230 ℃, 220～240 ℃, 230～240 ℃, 220～240 ℃, 230～240 ℃, head is 230～240 ℃; Extruding pelletization.At 100 ℃, the particle that obtains, after dry 3h, be injection molded into exemplar, standby survey, the temperature of injection moulding machine is 230～280 ℃.
Sample mechanical property is by following standard testing, and result is as shown in table 6: this matrix material not only has higher thermal conductivity, also has higher heat-drawn wire and good mechanical property.
Table 6
| Performance | Embodiment 6 | Inspecting standard |
| Density (g/cm 3) | 1.99 | ISO1183 |
| Tensile strength (Mpa) | 58 | ISO 527-1 |
| Flexural strength (Mpa) | 106 | ISO 178 |
| Charpy notched Izod impact strength (KJ/m 2) | 5 | ISO179-1 |
| Flame retardant properties (1.6mm) | V-0 | UL94 |
| Thermal conductivity (W/mK) | 1.5 | ASTME 1461-01 |
Embodiment 7
A kind of fire retardant insulating heat conduction polybutylene terephthalate matrix material, this matrix material is made up of the raw material of following component and weight part:
Wherein, PBT is middle low viscosity kind, and melting index is greater than 50g/10min (250 ℃, 2.16Kg); Heat conductive filler is the composite of silicon carbide and aluminum oxide; Oxidation inhibitor is the composite of Hinered phenols primary antioxidant and phosphorous acid esters auxiliary antioxidant; wherein: Hinered phenols primary antioxidant is N; N '-bis--(3-(3; 5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine (oxidation inhibitor 1098); phosphorous acid esters auxiliary antioxidant is 4; 4 '-[1,1 '-xenyl] subunit di 2 ethylhexyl phosphonic acid-tetra-[2,4-, bis-trimethylphenylmethane bases] ester (oxidation inhibitor PEPQ).
Coupling agent is titante coupling agent; Liquid adjuvants is commercially available white oil; Toughner is ethylene-methyl acrylate-glyceryl methacrylate terpolymer; Lubricant is silicone; Fire retardant is environmental protection bromide fire retardant brominated styrene; Fire retarding synergist is antimonous oxide.
A preparation method for fire retardant insulating heat conduction polybutylene terephthalate matrix material, the method comprises the following steps:
(1) after 0.5 part of coupling agent is mixed with 0.7 part of liquid adjuvants, join in 55 parts of dry heat conductive fillers, in high mixer, stir 30 minutes, for subsequent use after dry 3h at 100 ℃;
(2) by 37 parts of dry PBT, 0.3 part of oxidation inhibitor, 0.7 part of lubricant, 5.0 parts of toughner, 6.0 parts of fire retardants, 2.0 parts of fire retarding synergists and step (1) gains, put into high-speed mixer, stir after 15 minutes, put into forcing machine extruding pelletization.
Wherein, the mode that the coupling agent in step (1) and liquid adjuvants join in heat conductive filler adds for spraying; In step (1), dry heat conductive filler refers to the heat conductive filler after dry 4h at 80 ℃; In step (2), dry PBT refers to the PBT after dry 4h at 100 ℃.Forcing machine is the twin screw extruder of six sections of heating, and the temperature in 1 district～6 district is respectively: 170～190 ℃, 210～230 ℃, 230～250 ℃, 240～260 ℃, 240～260 ℃, 240～260 ℃, the head temperature of twin screw extruder is 230～250 ℃.
The above-mentioned description to embodiment is can understand and apply the invention for ease of those skilled in the art.Person skilled in the art obviously can easily make various modifications to these embodiment, and General Principle described herein is applied in other embodiment and needn't passes through performing creative labour.Therefore, the invention is not restricted to the embodiment here, those skilled in the art are according to announcement of the present invention, and not departing from the improvement that category of the present invention makes and revise all should be within protection scope of the present invention.
Claims (10)
1. a fire retardant insulating heat conduction polybutylene terephthalate matrix material, is characterized in that, this matrix material is made up of the component that comprises following weight part:
2. a kind of fire retardant insulating heat conduction polybutylene terephthalate matrix material according to claim 1, is characterized in that, described PBT is middle low viscosity kind, and melting index is greater than 50g/10min (250 ℃, 2.16Kg).
3. a kind of fire retardant insulating heat conduction polybutylene terephthalate matrix material according to claim 1, it is characterized in that, described heat conductive filler is selected from one or more in silicon carbide, aluminum oxide, boron nitride or aluminium nitride, preferably a kind of in silicon carbide or aluminum oxide or both is composite.
4. a kind of fire retardant insulating heat conduction polybutylene terephthalate matrix material according to claim 1; it is characterized in that; described oxidation inhibitor is the composite of Hinered phenols primary antioxidant and phosphorous acid esters auxiliary antioxidant; described Hinered phenols primary antioxidant is N; N '-bis--(3-(3; 5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine; described phosphorous acid esters auxiliary antioxidant is three [2.4-di-tert-butyl-phenyl] phosphorous acid ester or 4; 4 '-[1; 1 '-xenyl] subunit di 2 ethylhexyl phosphonic acid-tetra-[2,4-, bis-trimethylphenylmethane bases] ester.
5. a kind of fire retardant insulating heat conduction polybutylene terephthalate matrix material according to claim 1, is characterized in that, described coupling agent is selected from titante coupling agent or silane coupling agent, preferably γ-glycidyl ether oxygen propyl trimethoxy silicane.
6. a kind of fire retardant insulating heat conduction polybutylene terephthalate matrix material according to claim 1, is characterized in that, described liquid adjuvants is commercially available white oil.
7. a kind of fire retardant insulating heat conduction polybutylene terephthalate matrix material according to claim 1, is characterized in that, described toughner is ethylene-methyl acrylate-glyceryl methacrylate terpolymer.
8. a kind of fire retardant insulating heat conduction polybutylene terephthalate matrix material according to claim 1, is characterized in that, described lubricant is selected from silicone or pentaerythritol stearate; Described fire retardant is environmental protection bromide fire retardant, is selected from TDE or brominated styrene, preferably TDE; Described fire retarding synergist is antimonous oxide.
9. a preparation method for fire retardant insulating heat conduction polybutylene terephthalate matrix material as claimed in claim 1, is characterized in that, the method comprises the following steps:
(1) after 0.5～0.7 part of coupling agent is mixed with 0.5～0.7 part of liquid adjuvants, join in 55～67 parts of dry heat conductive fillers, in high mixer, stir 30 minutes, for subsequent use after dry 3h at 100 ℃;
(2) by 25～37 parts of dry PBT, 0.3～0.4 part of oxidation inhibitor, 0.5～0.7 part of lubricant, 2.0～5.0 parts of toughner, 3.0～6.0 parts of fire retardants, 1.0～2.0 parts of fire retarding synergists and step (1) gains, put into high-speed mixer, stir after 15 minutes, put into forcing machine extruding pelletization.
10. the preparation method of a kind of fire retardant insulating heat conduction polybutylene terephthalate matrix material according to claim 8, is characterized in that, the mode that the coupling agent in step (1) and liquid adjuvants join in heat conductive filler adds for spraying; In step (1), dry heat conductive filler refers to the heat conductive filler after dry 4h at 80 ℃; In step (2), dry PBT refers to the PBT after dry 4h at 100 ℃;
Described forcing machine is the twin screw extruder of six sections of heating, and the temperature in 1 district～6 district is respectively: 170～190 ℃, and 210～230 ℃, 230～250 ℃, 240～260 ℃, 240～260 ℃, 240～260 ℃, the head temperature of twin screw extruder is 230～250 ℃.
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