CN102604372B - Polyamide composite material with flame retardance and heat conduction and preparation method thereof - Google Patents
Polyamide composite material with flame retardance and heat conduction and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a polyamide composite material with flame retardance and heat conduction and a preparation method of the polyamide composite material. The polyamide composite material comprises the following components in percentage by weight: 30-70% of polyamide, 30-70% of modified compound graphite, 0.1-5% of a lubricant and 0.1-1% of an antioxidant; and the sum of the components is 100%. The preparation method of the polyamide composite material comprises the following steps of (1) adding the polyamide, the modified compound graphite, the lubricant and the antioxidant in a blending machine according to the proportion and blending for 5-10min; and (2) adding the mixed materials into a main feeding mouth of a double-screw extrusion machine, melting at a temperature of 230-260 DEG C and extruding for granulation. According to the polyamide composite material and the preparation method of the polyamide composite material, provided by the invention, magnesium hydroxide generated by an in-situ method is a good inorganic flame retardant, can act with expanded graphite together to endow the composite material with good flame retardant performance, can also play a role of coating, and improves the processing performance of graphite composite materials, and the composite material is good in flame retardance and heat conduction.
Description
Technical field
The present invention relates to a kind of polyamide-based matrix material and preparation method thereof, specifically a kind of polyamide compoiste material that has fire-retardant and heat conduction concurrently and preparation method thereof.
Background technology
Most polymers is all that inflammable material and thermal conductivity are lower, and polymkeric substance will reach fire-retardant purpose, and the most frequently used and easy method is to add wherein fire retardant, such as halogenated flame retardant, and organic phosphorus flame retardant, inorganic combustion inhibitor etc.Expansible black lead is a kind of novel expansion type flame retardant, is heated while reaching certain temperature, and due to occlusion compound decomposition in the interlayer dot matrix, expansible black lead just starts to expand, and in the time of 1000 ℃, expands fully, reaches maximum volume.When expanding volume can reach initial more than 200 times.Graphite after expansion is called expanded graphite or graphite worm, by former flakey, becomes the vermiform that density is very low, has formed an extraordinary thermal insulation layer, can be effectively heat insulation, there is rate of heat release low in fire, and mass loss is little, the characteristics that the flue gas of generation is few.Be widely used in polymer-based flame-proof composite material.Polymkeric substance will reach the purpose of heat conduction, and the most frequently used and easy approach is to add wherein heat conductive filler, such as metal powder, graphite, carbon black, metal oxide, carbon fiber, nitride, carbide etc.
Preparation has fire-retardant and polyamide compoiste material heat conduction concurrently, normally in polymeric amide, add fire retardant and heat conductive filler, owing to causing adding of a large amount of fire retardants and thermal conducting agent the mechanical property of material sharply to descend, the cost of product is also very high simultaneously, so its application is limited by very large.
Summary of the invention
Technical problem to be solved by this invention is: the shortcoming existed for above prior art, a kind of polyamide compoiste material that has fire-retardant and heat conduction concurrently and preparation method thereof is proposed, and matrix material is fire-retardant and heat conductivility is good.
The technical scheme that the present invention solves above technical problem is:
A kind ofly have fire-retardant and polyamide compoiste material heat conduction concurrently, its weight percent component is: polymeric amide: 30～70%, and the composite graphite of modification: 30～70%, lubricant: 0.1～5%, oxidation inhibitor: 0.1～1%; Above each component sum is 100%; The composite graphite of modification is comprised of modification expansible black lead and modified expanded graphite, and modification expansible black lead and modified expanded graphite weight proportion are: the modification expansible black lead: modified expanded graphite is 1:1～3:1;
The preparation technology of modification expansible black lead is:
1. prepare magnesium chloride solution and alkaline solution: the solid content of magnesium chloride solution and alkaline solution is 10～60%;
2. coat to process expansible black lead: expansible black lead is added in the magnesium chloride solution that 1. step prepare, the alkaline solution that adds step 1. to prepare after stirring, after magnesium solution to be chlorinated and alkaline solution react completely, standing, suction filtration, use deionized water wash 5-6 time, suction filtration, oven dry obtains the expansible black lead of coat processing, and described magnesium chloride solution and alkaline solution weight sum are the polyamide compoiste material weight that will make 50～90%, and described magnesium chloride solution and alkaline solution weight ratio are 1:1;
3. coupling processing expansible black lead: expansible black lead and coupling agent that the coating that 2. step is obtained is processed add in blender, at 50-90 ℃ of lower blend 5-10min, obtain the modification expansible black lead, the 0.5-5% that described coupling agent add-on is the expansible black lead weight processed of the coating that 2. obtains of step;
The preparation technology of modified expanded graphite is:
(1) prepare magnesium chloride solution and alkaline solution: the solid content of magnesium chloride solution and alkaline solution is 10～60%;
(2) coat to process expanded graphite: expanded graphite is added in the magnesium chloride solution that (1) step prepare, the alkaline solution that adds step (1) to prepare after stirring, after magnesium solution to be chlorinated and alkaline solution react completely, standing, suction filtration, use deionized water wash 5-6 time, suction filtration, oven dry obtains the expanded graphite of coat processing, and described magnesium chloride solution and alkaline solution weight sum are the polyamide compoiste material weight that will make 10～50%, and described magnesium chloride solution and alkaline solution weight ratio are 1:1;
(3) coupling processing expanded graphite: expanded graphite and coupling agent that the coating that 2. step is obtained is processed add in blender, at 50-90 ℃ of lower blend 5-10min, obtain modified expanded graphite, the 0.5-5% that described coupling agent add-on is the expanded graphite weight processed of the coating that (2) obtains of step;
The preparation technology of the composite graphite of modification is: modification expansible black lead and modified expanded graphite are added in blender according to above proportioning, at 50-90 ℃ of lower blend 5-10min, obtain the composite graphite of modification.
The aforementioned preparation method who has the polyamide compoiste material of fire-retardant and heat conduction concurrently comprises the following steps:
(i) polymeric amide, the composite graphite of modification, lubricant and oxidation inhibitor are added in blender to blend 5-10min according to above proportioning;
(ii) the material mixed is joined to the main spout of twin screw extruder, under 230-260 ℃, melt extrude granulation.
Expansible black lead is natural flake graphite (or the very high electrographite of degree of graphitization), and the intercalation compound after acidic oxidation agent (sulfuric acid, nitric acid and hydrogen peroxide, potassium permanganate) is processed, also claim graphite oxide.The immersion of oxygenant, also make original graphite produce the small expansion behavior, and interlamellar spacing increases to 6-11A by original 3.35A.The graphite oxide key property is that unusual swelling property is arranged, and can at high temperature expand, therefore be expansible black lead.
Expanded graphite is that graphite oxide is at 960-980 ℃ of high temperature action, the decomposition of gasifying rapidly of the compound of graphite layers, produce a certain amount of thrust, destroy the molecular force of graphite layers combination, make the C-C bond rupture of graphite wafer compartment, aspect expands rapidly along the c-axis direction, and interlamellar spacing increases 50-500 doubly, by flaky graphite more closely, become fine cotton-shaped type quasiflake graphite.
What the present invention adopted is that a kind of " original position " reaction generates the method that magnesium hydroxide coats expansible black lead and expanded graphite, the expansible black lead coated through magnesium hydroxide and expanded graphite have higher tap density than expansible black lead and the expanded graphite mixture before not coating, the density of two kinds of graphite is close, consistency is better, again after coupling processing, with polyamide substrate, good consistency is arranged, while preparing polyamide compoiste material, blanking and dispersion are more easy, have improved the processing characteristics of graphite composite material.Expansible black lead is a kind of expansion type flame retardant, is widely used in flame-proof composite material; Magnesium hydroxide is a kind of inorganic combustion inhibitor, it and expansible black lead acting in conjunction, the good flame retardant effect of performance in matrix material.After the verified and polymeric amide of expanded graphite prepares matrix material, the capacity of heat transmission of polyamide compoiste material obviously improves, and just because the expanded graphite surface is fluffy, blanking and dispersion are all more difficult, caused a very large processing difficult problem, so just be not widely used.The method of " original position " inorganic particulate coating graphite that the present invention adopts has solved this difficult problem well.
Characteristics of the present invention are that the expansible black lead of selecting is fire retardant, it is again good thermal conducting agent, prepare so the total amount of filler of flame-retarded heat-conducting polyamide compoiste material and just reduced, the mechanical property of material can not reduce because of too much filler, has reduced cost prepared by matrix material simultaneously yet; The magnesium hydroxide that " original position " method generates is good inorganic combustion inhibitor, the flame retardant properties of matrix material excellence is given in energy and expansible black lead acting in conjunction, can play coating function again, improve the processing characteristics of graphite composite material, also there is certain thermal conductivity simultaneously; Add a small amount of expanded graphite can obviously improve the heat conductivility of material.
The technical scheme that the present invention further limits is:
Aforesaidly have fire-retardant and polyamide compoiste material heat conduction concurrently, polymeric amide is a kind of in heat-resistant polyamide, PA6 or PA66 or mixes.
Aforesaidly have fire-retardant and polyamide compoiste material heat conduction concurrently, the expansible black lead expansion multiplying power is 50-400 mL/g, and initial expansion temperature is greater than 300 ℃, and carbon content is more than 98%.
Aforesaidly have fire-retardant and polyamide compoiste material heat conduction concurrently, lubricant is stearate, stearic amide, low-molecular(weight)polymer or paraffin.
Aforesaidly have fire-retardant and polyamide compoiste material heat conduction concurrently, oxidation inhibitor is phenols or one or more mixtures of phosphorous acid esters.
Aforesaidly have fire-retardant and polyamide compoiste material heat conduction concurrently, coupling agent is silane coupling agent, titanate coupling agent or aluminate coupling agent.
Embodiment
Embodiment 1
A kind ofly have fire-retardant and polyamide compoiste material heat conduction concurrently, its weight percent component is:
PA6：69%，
The composite graphite 30% of modification, wherein the expansible black lead expansion multiplying power is 50 mL/g, and initial expansion temperature is greater than 300 ℃, and carbon content is 99%,
Paraffin: 1%;
Oxidation inhibitor: 1010(0.1%), 168(0.15%), add-on is 0.1% and 0.15% of PA6, the composite graphite of modification and paraffin total amount.
Have the preparation method of the polyamide compoiste material of fire-retardant and heat conduction concurrently, comprise the following steps:
The composite graphite of modification: 1. prepare magnesium chloride solution and sodium hydroxide solution: the magnesium chloride brine solid content is 16.4%, and the solid content of sodium hydroxide water is 13.8%; 2. coat to process expansible black lead: by 75%(polyamide compoiste material weight 75%) magnesium chloride solution and 75%(polyamide compoiste material weight 75%) sodium hydroxide solution join expansible black lead after stirring reaction after for some time, standing, suction filtration, deionized water wash 5-6 time, suction filtration, dry under 100 ℃ and obtain coating the expansible black lead of processing; 3. coat to process expanded graphite: after the magnesium chloride solution by 25% and 25% sodium hydroxide solution join expanded graphite, stirring reaction is after for some time, standing, suction filtration, and deionized water wash 5-6 time, suction filtration, dry the expanded graphite that obtains coating processing under 100 ℃; 4. coupling processing expanded graphite: will coat expanded graphite after processing and 1% titanate coupling agent and add in the high speed blender, and at 80 ℃ of lower blend 10min, obtain modified expanded graphite; Adopt identical method to obtain the modification expansible black lead; By modification expansible black lead and modified expanded graphite by weight ratio 3:1 add in the high speed blender, blend 5min obtains the composite graphite of modification, standby;
Material premix: polyamide substrate resin, the composite graphite of modification, paraffin and oxidation inhibitor are added to blend 5min in the high speed blender by above proportioning;
Granulation: the material mixed is added to the main spout of twin screw extruder, at 250 ℃, melt extrude granulation.
Embodiment 2
A kind ofly have fire-retardant and polyamide compoiste material heat conduction concurrently, its weight percent component is:
PA6：64%，
The composite graphite of modification: 35%, wherein the expansible black lead expansion multiplying power is 100 mL/g, and initial expansion temperature is greater than 300 ℃, and carbon content is 99%,
Paraffin: 1%;
Oxidation inhibitor: 1010(0.15%), 168(0.35%), add-on is 0.15% and 0.35% of PA6, the composite graphite of modification and paraffin total amount.
Have the preparation method of the polyamide compoiste material of fire-retardant and heat conduction concurrently, comprise the following steps:
The composite graphite of modification: 1. prepare magnesium chloride solution and sodium hydroxide solution: the magnesium chloride brine solid content is 16.4%, and the solid content of sodium hydroxide water is 13.8%; 2. coat to process expansible black lead: by 60%(polyamide compoiste material weight 60%) magnesium chloride solution and 60%(polyamide compoiste material weight 60%) sodium hydroxide solution join expansible black lead after stirring reaction after for some time, standing, suction filtration, deionized water wash 5-6 time, suction filtration, dry under 100 ℃ and obtain coating the expansible black lead of processing; 3. coat to process expanded graphite: by 40%(polyamide compoiste material weight 40%) magnesium chloride solution and 40%(polyamide compoiste material weight 40%) sodium hydroxide solution join expansible black lead after stirring reaction after for some time, standing, suction filtration, deionized water wash 5-6 time, suction filtration, dry under 100 ℃ and obtain coating the expanded graphite of processing; 4. coupling processing expanded graphite: will coat expanded graphite after processing and 1% titanate coupling agent and add in the high speed blender, and at 80 ℃ of lower blend 10min, obtain modified expanded graphite; Adopt identical method to obtain the modification expansible black lead; Modification expansible black lead and modified expanded graphite are added in the high speed blender by weight 3:2, and blend 5min obtains the composite graphite of modification, standby.
Material premix: polyamide substrate resin, the composite graphite of modification, paraffin and oxidation inhibitor are added to blend 5min in the high speed blender by above proportioning.
Granulation: the material mixed is added to the main spout of twin screw extruder, at 250 ℃, melt extrude granulation.
Embodiment 3
A kind ofly have fire-retardant and polyamide compoiste material heat conduction concurrently, its weight percent component is:
PA6：53.5%，
The composite graphite 45% of modification, wherein the expansible black lead expansion multiplying power is 200 mL/g, and initial expansion temperature is greater than 300 ℃, and carbon content is 99%,
Paraffin: 1.5%;
Oxidation inhibitor: 1010(0.35%), 168(0.55%), add-on is 0.35% and 0.55% of PA6, the composite graphite of modification and paraffin total amount.
Have the preparation method of the polyamide compoiste material of fire-retardant and heat conduction concurrently, comprise the following steps:
The composite graphite of modification: 1. prepare magnesium chloride solution and sodium hydroxide solution: the magnesium chloride brine solid content is 16.4%, and the solid content of sodium hydroxide water is 13.8%; 2. coat to process expansible black lead: by 50%(polyamide compoiste material weight 50%) magnesium chloride solution and 50%(polyamide compoiste material weight 50%) sodium hydroxide solution join expansible black lead after stirring reaction after for some time, standing, suction filtration, deionized water wash 5-6 time, suction filtration, dry under 100 ℃ and obtain coating the expansible black lead of processing; 3. coat to process expanded graphite: by 50%(polyamide compoiste material weight 50%) magnesium chloride solution and 50%(polyamide compoiste material weight 50%) sodium hydroxide solution join expansible black lead after stirring reaction after for some time, standing, suction filtration, deionized water wash 5-6 time, suction filtration, dry under 100 ℃ and obtain coating the expanded graphite of processing; 4. coupling processing expanded graphite: will coat expanded graphite after processing and 1% titanate coupling agent and add in the high speed blender, and at 80 ℃ of lower blend 10min, obtain modified expanded graphite; Coupling processing expanded graphite: will coat expansible black lead after processing and 1.5% titanate coupling agent and add in the high speed blender, and at 80 ℃ of lower blend 10min, obtain the modification expansible black lead; Modification expansible black lead and modification expansible black lead are added in the high speed blender by weight 5:2, at 80 ℃ of lower blend 5min, obtain the composite graphite of modification, standby;
Material premix: polyamide substrate resin, the composite graphite of modification, paraffin and oxidation inhibitor are added to blend 5min in the high speed blender by above proportioning;
Granulation: the material mixed is added to the main spout of twin screw extruder, under 250 ℃, melt extrude granulation.
Embodiment 4
A kind ofly have fire-retardant and polyamide compoiste material heat conduction concurrently, its weight percent component is:
PA6：43%，
The composite graphite 55% of modification, wherein the expansible black lead expansion multiplying power is 300 mL/g, and initial expansion temperature is greater than 300 ℃, and carbon content is 99%,
Paraffin: 2%;
Oxidation inhibitor: 1010(0.1%), 168(0.15%), add-on is 0.1% and 0.15% of PA6, the composite graphite of modification and paraffin total amount.
Have the preparation method of the polyamide compoiste material of fire-retardant and heat conduction concurrently, comprise the following steps:
The composite graphite of modification: 1. prepare magnesium chloride solution and sodium hydroxide solution: the magnesium chloride brine solid content is 32.7%, and the solid content of sodium hydroxide water is 27.6%; 2. coat to process expansible black lead: by 70%(polyamide compoiste material weight 70%) magnesium chloride solution and 70%(polyamide compoiste material weight 70%) sodium hydroxide solution join expansible black lead after stirring reaction after for some time, standing, suction filtration, deionized water wash 5-6 time, suction filtration, dry under 100 ℃ and obtain coating the expansible black lead of processing; 3. coat to process expanded graphite: by 30%(polyamide compoiste material weight 30%) magnesium chloride solution and 30%(polyamide compoiste material weight 30%) sodium hydroxide solution join expansible black lead after stirring reaction after for some time, standing, suction filtration, deionized water wash 5-6 time, suction filtration, dry under 100 ℃ and obtain coating the expanded graphite of processing; 4. coupling processing expanded graphite: will coat expanded graphite after processing and 1% titanate coupling agent and add in the high speed blender, and at 80 ℃ of lower blend 10min, obtain modified expanded graphite; Adopt identical method to obtain modification expansible black lead (2% titanate coupling agent); Modification expansible black lead and modified expanded graphite are added in the high speed blender by weight 5:2, at 80 ℃ of lower blend 5min, obtain the composite graphite of modification, standby;
Material premix: the admixed graphite after polyamide substrate resin, modification, paraffin and oxidation inhibitor are added to blend 5min in the high speed blender by above proportioning;
Granulation: the material mixed is added to the main spout of twin screw extruder, under 250 ℃, melt extrude granulation.
Embodiment 5
A kind ofly have fire-retardant and polyamide compoiste material heat conduction concurrently, its weight percent component is:
PA6：37%，
The composite graphite 60% of modification, wherein the expansible black lead expansion multiplying power is 350mL/g, and initial expansion temperature is greater than 300 ℃, and carbon content is 99%,
Paraffin: 3%;
Oxidation inhibitor: 1010(0.1%), 168(0.15%), add-on is 0.1% and 0.15% of PA6, the composite graphite of modification and paraffin total amount.
Have the preparation method of the polyamide compoiste material of fire-retardant and heat conduction concurrently, comprise the following steps:
The composite graphite of modification: 1. prepare magnesium chloride solution and sodium hydroxide solution: the magnesium chloride solution solid content is 32.7%, and the solid content of sodium hydroxide solution is 27.6%; 2. coat to process expansible black lead: by 75%(polyamide compoiste material weight 75%) magnesium chloride solution and 75%(polyamide compoiste material weight 75%) sodium hydroxide solution join expansible black lead after stirring reaction after for some time, standing, suction filtration, deionized water wash 5-6 time, suction filtration, dry under 100 ℃ and obtain coating the expansible black lead of processing; 3. coat to process expanded graphite: after the magnesium chloride solution by 25% (polyamide compoiste material weight 25%) and 25% sodium hydroxide solution (polyamide compoiste material weight 25%) join expansible black lead, stirring reaction is after for some time, standing, suction filtration, deionized water wash 5-6 time, suction filtration, dry under 100 ℃ and obtain coating the expanded graphite of processing; 4. coupling processing expanded graphite: will coat expanded graphite after processing and 1% titanate coupling agent and add in the high speed blender, and at 80 ℃ of lower blend 10min, obtain modified expanded graphite; Adopt identical method to obtain modification expansible black lead (2% titanate coupling agent); Modification expansible black lead and modified expanded graphite are added in the high speed blender by weight 3:1, at 80 ℃ of lower blend 5min, obtain the composite graphite of modification, standby;
Material premix: polyamide substrate resin, the composite graphite of modification, paraffin and oxidation inhibitor are added to blend 5min in the high speed blender by above proportioning;
Granulation: the material mixed is added to the main spout of twin screw extruder, under 250 ℃, melt extrude granulation.
Embodiment 6
A kind ofly have fire-retardant and polyamide compoiste material heat conduction concurrently, its weight percent component is:
PA6：25%，
The composite graphite 70% of modification, wherein the expansible black lead expansion multiplying power is 400 mL/g, and initial expansion temperature is greater than 300 ℃, and carbon content is 99%,
Paraffin: 5%
Oxidation inhibitor: 1010(0.1%), 168(0.15%), add-on is 0.1% and 0.15% of PA6, the composite graphite of modification and paraffin total amount.
Have the preparation method of the polyamide compoiste material of fire-retardant and heat conduction concurrently, comprise the following steps:
The composite graphite of modification: 1. prepare magnesium chloride solution and sodium hydroxide solution: the magnesium chloride solution solid content is 49.2%, and the solid content of sodium hydroxide solution is 41.4%; 2. coat to process expansible black lead: by 75%(polyamide compoiste material weight 75%) magnesium chloride solution and 75%(polyamide compoiste material weight 75%) sodium hydroxide solution join expansible black lead after stirring reaction after for some time, standing, suction filtration, deionized water wash 5-6 time, suction filtration, dry under 100 ℃ and obtain coating the expansible black lead of processing; 3. coat to process expanded graphite: by 25%(polyamide compoiste material weight 25%) magnesium chloride solution and 25%(polyamide compoiste material weight 25%) sodium hydroxide solution join expansible black lead after stirring reaction after for some time, standing, suction filtration, deionized water wash 5-6 time, suction filtration, dry under 100 ℃ and obtain coating the expanded graphite of processing; 4. coupling processing expanded graphite: will coat expanded graphite after processing and 1% titanate coupling agent and add in the high speed blender, and at 80 ℃ of lower blend 10min, obtain modified expanded graphite; Adopt identical method to obtain modification expansible black lead (2.5% titanate coupling agent); Modification expansible black lead and modified expanded graphite are added in the high speed blender by weight 3:1, at 80 ℃ of lower blend 5min, obtain the composite graphite of modification, standby;
Material premix: polyamide substrate resin, the composite graphite of modification, paraffin and oxidation inhibitor are added to blend 5min in the high speed blender by above proportioning;
Granulation: the material mixed is added to the main spout of twin screw extruder, at 250 ℃, melt extrude granulation.
The parameter testing of above embodiment the results are shown in Table 1:
Table 1
The present invention can also have other embodiment, and the technical scheme that the equal replacement of all employings or equivalent transformation form, within all dropping on the scope of protection of present invention.
Claims (7)
1. one kind has fire-retardant and polyamide compoiste material heat conduction concurrently, and it is characterized in that: its weight percent component is: polymeric amide: 30～70%, and the composite graphite of modification: 30～70%, lubricant: 0.1～5%, oxidation inhibitor: 0.1～1%; Above each component sum is 100%; The composite graphite of described modification is comprised of modification expansible black lead and modified expanded graphite, and described modification expansible black lead and modified expanded graphite weight proportion are: the modification expansible black lead: modified expanded graphite is 1:1～3:1;
The preparation technology of described modification expansible black lead is:
1. prepare magnesium chloride solution and sodium hydroxide solution: the solid content of magnesium chloride solution and sodium hydroxide solution is 10～60%;
2. coat to process expansible black lead: expansible black lead is added in the magnesium chloride solution that 1. step prepare, the alkaline solution that adds step 1. to prepare after stirring, after magnesium solution to be chlorinated and alkaline solution react completely, standing, suction filtration, use deionized water wash 5-6 time, suction filtration, oven dry obtains the expansible black lead of coat processing, and described magnesium chloride solution and alkaline solution weight sum are the polyamide compoiste material weight that will make 50～90%, and described magnesium chloride solution and alkaline solution weight ratio are 1:1;
3. coupling processing expansible black lead: expansible black lead and coupling agent that the coating that 2. step is obtained is processed add in blender, at 50-90 ℃ of lower blend 5-10min, obtain the modification expansible black lead, the 0.5-5% that described coupling agent add-on is the expansible black lead weight processed of the coating that 2. obtains of step;
The preparation technology of described modified expanded graphite is:
(1) prepare magnesium chloride solution and alkaline solution: the solid content of magnesium chloride solution and alkaline solution is 10～60%;
(2) coat to process expanded graphite: expanded graphite is added in the magnesium chloride solution that (1) step prepare, the alkaline solution that adds step (1) to prepare after stirring, after magnesium solution to be chlorinated and alkaline solution react completely, standing, suction filtration, use deionized water wash 5-6 time, suction filtration, oven dry obtains the expanded graphite of coat processing, and described magnesium chloride solution and alkaline solution weight sum are the polyamide compoiste material weight that will make 10～50%, and described magnesium chloride solution and alkaline solution weight ratio are 1:1;
(3) coupling processing expanded graphite: expanded graphite and coupling agent that the coating that (2) step is obtained is processed add in blender, at 50-90 ℃ of lower blend 5-10min, obtain modified expanded graphite, the 0.5-5% that described coupling agent add-on is the expanded graphite weight processed of the coating that (2) obtains of step;
The preparation technology of the composite graphite of described modification is: modification expansible black lead and modified expanded graphite are added in blender according to above proportioning, at 50-90 ℃ of lower blend 5-10min, obtain the composite graphite of modification.
2. as claimed in claim 1ly have fire-retardant and polyamide compoiste material heat conduction concurrently, it is characterized in that: described polymeric amide is a kind of in heat-resistant polyamide, PA6 or PA66 or mixes.
3. as claimed in claim 1ly have fire-retardant and polyamide compoiste material heat conduction concurrently, it is characterized in that: described expansible black lead expansion multiplying power is 50-400 mL/g, and initial expansion temperature is greater than 300 ℃, and carbon content is more than 98%.
4. as claimed in claim 1ly have fire-retardant and polyamide compoiste material heat conduction concurrently, it is characterized in that: described lubricant is stearate, stearic amide, low-molecular(weight)polymer or paraffin.
5. as claimed in claim 1ly have fire-retardant and polyamide compoiste material heat conduction concurrently, it is characterized in that: described oxidation inhibitor is phenols or one or more mixtures of phosphorous acid esters.
6. as claimed in claim 1ly have fire-retardant and polyamide compoiste material heat conduction concurrently, it is characterized in that: described coupling agent is silane coupling agent, titanate coupling agent or aluminate coupling agent.
7. the described preparation method who has the polyamide compoiste material of fire-retardant and heat conduction concurrently of claim 1 is characterized in that: comprise the following steps:
(i) polymeric amide, the composite graphite of modification, lubricant and oxidation inhibitor are added in blender to blend 5-10min according to the described proportioning of claim 1;
(ii) the material mixed is joined to the main spout of twin screw extruder, under 230-260 ℃, melt extrude granulation.
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