A kind of halogen-free flame retardant insulation heat conduction nylon and preparation method thereofTechnical field
The present invention relates to field of polymer material preparing technology, specifically a kind of halogen-free flame retardant insulation heat conduction nylon and preparation method thereof.
Background technology
Heat-conducting polymer material, as the novel thermally conductive material with good over-all properties of a class, substitutes traditional metal and pottery in many aspects, is widely used in the fields such as electronics, LED illumination, automobile, machinery.Heat-conducting polymer material beams back vital role in modern high-tech field because of its heat conduction, corrosion-resistant, good impact property, the advantage such as easy to process.Existing heat-conducting polymer material is filling-type thermal-conducting electric-insulating polymkeric substance mainly, refers to and is blended in insulating resin by heat conductive insulating inorganic filler particle, improves the heat conductivility of polymkeric substance, retains its electrical insulating property.
In the manufacturing of common heat-conducting plastic, use screw machine to carry out extruding and injection molding.Due to the ceramic powder that current most heat conductive filler is high rigidity, as aluminum oxide, silicon carbide, aluminium nitride, magnesium oxide etc., and addition is high, if add fire retardant again, loading level is very large, and this brings very large difficulty with regard to giving the processing of heat-conducting plastic, and causes heat-conducting plastic mechanical property degradation, and traditional way brings serious wearing and tearing to equipment, significantly limit the dosage range of heat-conducting plastic.
Therefore, find and a kind ofly can reduce processing units wearing and tearing, possess the preparation method of the flame-retarded heat-conducting engineering plastics of good mechanical property simultaneously, to the application of expanding insulating and heat-conducting plastics, in the prolonged mechanical processing units life-span, the popularization LED light source illumination New Times etc. is of practical significance.
Summary of the invention
For above-mentioned Problems existing, the object of the present invention is to provide a kind of halogen-free flame retardant insulation heat conduction nylon.
Another object of the present invention is to the preparation method that above-mentioned halogen-free flame retardant insulation heat conduction nylon is provided.
The present invention for achieving the above object, takes following technical scheme to be achieved:
A kind of halogen-free flame retardant insulation heat conduction nylon, comprises the following component of parts by weight:
Nylon: 100 parts;
Magnesium oxide: 50 ~ 150 parts;
Magnesium hydroxide: 100 ~ 150 parts;
Other processing aids: 0 ~ 5 part.
The screening formulation of a kind of halogen-free flame retardant insulation of the present invention heat conduction nylon is as follows: the following component comprising parts by weight:
Nylon: 100 parts;
Magnesium oxide: 75 ~ 120 parts;
Magnesium hydroxide: 100 ~ 150 parts;
Other processing aids: 0 ~ 5 part.
Preferably, also wollastonite fibre is comprised in above-mentioned formula: 5 ~ 30 parts.Wollastonite fibre belongs to mineral filler, does not substantially affect heat conduction, but can play obvious strengthening action, improves the mechanical property of nylon further.
Preferably, other processing aids described comprise oxidation inhibitor, lubricant and thermo-stabilizer, and the mass ratio of described oxidation inhibitor, lubricant and thermo-stabilizer is 2:1:2.
Preferably, described oxidation inhibitor is four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester and three [2.4-di-tert-butyl-phenyl] phosphorous acid ester, described lubricant is ethylene bis stearamide, and described thermo-stabilizer is N, N '-two (2,2,6,6-tetramethyl--4-piperidyl)-1,3-benzene diamide; Wherein, [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, three [2.4-di-tert-butyl-phenyl] phosphorous acid ester, ethylene bis stearamide and N, N '-two (2,2,6,6-tetramethyl--4-piperidyl) mass ratio of-1,3-benzene diamide is 1:1:2:1.
Preferably, described nylon is polyamide 6, and relative viscosity is 2.0-2.8.
Preferably, described magnesium oxide is through amino silicane coupling agent Surface coating activation treatment, and particle diameter is at 5 ~ 100 microns.
Preferably, described magnesium hydroxide is through amino silicane coupling agent Surface coating activation treatment, and particle diameter is at 2 ~ 20 microns.
Preferably, the length-to-diameter ratio of described wollastonite fibre is 10 ~ 20:1.
Another object of the present invention is to the preparation method of openly a kind of above-mentioned halogen-free flame retardant insulation heat conduction nylon, adopt the parallel dual-screw extruding machine possessing main charging opening and side-feed, comprise the following steps:
(1) according to formula feeding;
(2) by after nylon drying treatment, add magnesium hydroxide and other processing aids, stir, add parallel dual-screw extruding machine from main charging opening; Meanwhile, by magnesium oxide and wollastonite fibre from the side charging opening add parallel dual-screw extruding machine; Extrusion temperature be 225 ~ 260 DEG C, screw speed extrudes under being the condition of 200 ~ 260r/min and obtains halogen-free flame retardant insulation heat conduction nylon.
Compared with prior art, beneficial effect of the present invention is as follows:
(1) desirable thermal conductivity to be reached for existing heat conductive filler, high and the problem of mechanical property degradation of addition, the present invention is directed to heat conductive filler magnesium oxide, add magnesium hydroxide as fire retardant, nylon is not only made to reach the effect of halogen-free flameproof, also serve the effect of mutual cooperative flame retardant heat conduction with magnesium oxide, reduce the addition of filler, make material keep good mechanical property.
(2) in preparation method of the present invention, there is higher hardness, the magnesium oxide easily worn and torn and wollastonite fibre add from forcing machine side-feed, decrease the direct wearing and tearing of raw material to equipment, better maintain the length-to-diameter ratio of wollastonite fibre, the finished product are of light color, have good over-all properties.
Accompanying drawing explanation
Fig. 1 is the structural representation of the parallel dual-screw extruding machine possessing main charging opening and side-feed in the present invention.
Embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated.
Embodiment 1 ~ 6:
Halogen-free flame retardant insulation heat conduction nylon formula of the present invention is as shown in table 1:
Table 1 halogen-free flame retardant insulation heat conduction nylon (parts by weight)
Wherein, other processing aids comprise oxidation inhibitor, lubricant and thermo-stabilizer, and the mass ratio of oxidation inhibitor, lubricant and thermo-stabilizer is preferably 2:1:2.
Oxidation inhibitor is four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (antioxidant 1010) and three [2.4-di-tert-butyl-phenyl] phosphorous acid ester (irgasfos 168), described lubricant is ethylene bis stearamide, described thermo-stabilizer is N, N '-two (2,2,6,6-tetramethyl--4-piperidyl)-1,3-benzene diamide (SEED); Wherein, [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, three [2.4-di-tert-butyl-phenyl] phosphorous acid ester, ethylene bis stearamide and N, N '-two (2,2,6,6-tetramethyl--4-piperidyl) mass ratio of-1,3-benzene diamide is 1:1:2:1.
Nylon is polyamide 6, and relative viscosity is 2.0-2.8.
Magnesium oxide is through amino silicane coupling agent Surface coating activation treatment, and particle diameter is at 5 ~ 100 microns.
Magnesium hydroxide is through amino silicane coupling agent Surface coating activation treatment, and particle diameter is at 2 ~ 20 microns.
Wollastonite fibre belongs to mineral filler, does not substantially affect heat conduction, but can play obvious strengthening action, improves the mechanical property of nylon further.In embodiment, the length-to-diameter ratio of wollastonite fibre is 10 ~ 20:1.
Embodiment 7
Prepare halogen-free flame retardant insulation heat conduction nylon according to formula described in embodiment 1-6, this preparation method adopts the parallel dual-screw extruding machine possessing main charging opening 1# and side-feed 2#, see Fig. 1, comprises the following steps:
(1) according to formula feeding;
(2) by after nylon drying treatment, add magnesium hydroxide and other processing aids, stir, add parallel dual-screw extruding machine from main charging opening; Meanwhile, by magnesium oxide and wollastonite fibre from the side charging opening add parallel dual-screw extruding machine; Extrusion temperature be 225 ~ 260 DEG C, screw speed extrudes under being the condition of 200 ~ 260r/min and obtains halogen-free flame retardant insulation heat conduction nylon, is designated as finished product sample 1-6.
Preferably, as shown in Figure 1, setting 1 district's temperature is 225 ~ 235 DEG C, and 2 district's temperature are 235 ~ 255 DEG C, 3 district's temperature are 235 ~ 255 DEG C, 4 district's temperature are 240 ~ 260 DEG C, and 5 district's temperature are 240 ~ 260 DEG C, and 6 district's temperature are 240 ~ 260 DEG C, 7 district's temperature are 240 ~ 260 DEG C, 8 district's temperature are 240 ~ 260 DEG C, and 9 district's temperature are 230 ~ 250 DEG C, head temperature 240 ~ 260 DEG C; Setting screw speed 200 ~ 260n/min, through extruding blended, cooling, granulation, obtains halogen-free flame retardant insulation heat conduction nylon.
In preparation method of the present invention, there is higher hardness, the magnesium oxide easily worn and torn and wollastonite fibre add from forcing machine side-feed, decrease the direct wearing and tearing of raw material to equipment, better maintain the length-to-diameter ratio of wollastonite fibre, the finished product are of light color, have good over-all properties.
In addition, comparative example formula described in table 2 is extruded according to the method described above obtain comparative sample 1-6.
Table 2 comparative example formula (parts by weight)
By finished product sample 1-6, comparative sample 1-6 respectively through injection moulding test performance, the performance test results is in table 3 ~ 4:
Table 3 halogen-free reinforced nylon detection perform table
Table 4 comparative example detection perform table
As shown in table 2 and 4: only with the addition of magnesium oxide in comparative example 1 ~ 3, along with the increase of magnesium oxide addition, thermal conductivity increases thereupon; Do not possess flame-retarding characteristic; The intensity of material and heat-drawn wire are all lower.Only with the addition of magnesium hydroxide in comparative example 4 ~ 6, along with the increase of magnesium hydroxide addition, flame retardant effect increases; Intensity and heat-drawn wire higher; Even if but addition reaches 150 parts, the thermal conductivity of material is also lower.
As shown in table 1 and 3: when to add magnesium oxide and magnesium hydroxide simultaneously, matrix material has not only possessed good thermal conduction characteristic and good comprehensive mechanical performance, and reaches UL94V0 flame retardant rating.Magnesium hydroxide and magnesium oxide serve the effect of mutual cooperative flame retardant heat conduction, reduce magnesian addition, make material keep good mechanical property.The present invention effectively can solve the thermal conductivity that existing heat conductive filler will reach desirable, the high and problem of mechanical property degradation of addition.
In addition, because magnesium hydroxide is a kind of environment friendly halogen-free fireproof agent, the environmental protection more of traditional Halogen fire retardant material compared by therefore obtained heat conduction nylon.
See table 1 and 3, acicular wollastonite, as a kind of auxiliary packing, when keeping product heat conduction and flame-retarding characteristic is substantially constant, makes the intensity of material and heat-drawn wire all increase.
Above the technical scheme that the embodiment of the present invention provides is described in detail, apply specific case herein to set forth the principle of the embodiment of the present invention and embodiment, the explanation of above embodiment is only applicable to the principle helping to understand the embodiment of the present invention; Meanwhile, for one of ordinary skill in the art, according to the embodiment of the present invention, embodiment and range of application all will change, and in sum, this description should not be construed as limitation of the present invention.