阅读说明：本技术 一种抗静电聚酰胺复合材料及其制备方法 (A kind of static resistant polyamide composite material and preparation method ) 是由 杨桂生 赵冬云 严莉莉 李兰杰 于 2018-05-22 设计创作，主要内容包括：本发明提供了一种抗静电聚酰胺复合材料,其生产原料包括：脂肪族/芳香族二元酸20-80份,含磺酸盐基团的二元酸0.2-10份,脂肪族二元胺20-80份,石墨烯水溶液2-30份,封端剂0.1-0.4份,催化剂0.01-0.06份,去离子水30-160份。本发明还提供了该复合材料的制备方法。本发明制备的抗静电聚酰胺复合材料具有良好的抗静电性能、较好的力学性能、优异的相容性、较好的耐热性能和较高的热变形温度,扩大了其应用范围,还降低了生产成本。(The present invention provides a kind of static resistant polyamide composite materials, its raw materials for production includes: 20-80 parts of aliphatic/aromatic binary acid, 0.2-10 parts of binary acid containing sulfonate groups, 20-80 parts of aliphatic diamine, 2-30 parts of graphene aqueous solution, 0.1-0.4 parts of end-capping reagent, 0.01-0.06 parts of catalyst, 30-160 parts of deionized water.The present invention also provides the preparation methods of the composite material.Static resistant polyamide composite material prepared by the present invention has good antistatic property, preferable mechanical property, excellent compatibility, preferable heat resistance and higher heat distortion temperature, expands its application range, also reduces production cost.)

1. a kind of static resistant polyamide composite material, it is characterised in that: its raw materials for production comprises the following components in parts by weight:

20-80 parts of aliphatic/aromatic binary acid,

0.2-10 parts of binary acid containing sulfonate groups,

20-80 parts of aliphatic diamine,

2-30 parts of graphene aqueous solution,

0.1-0.4 parts of end-capping reagent,

0.01-0.06 parts of catalyst,

30-160 parts of deionized water.

2. static resistant polyamide composite material according to claim 1, it is characterised in that: the aliphatic/aromatic two First acid is 30-60 parts；And/or

The binary acid containing sulfonate groups is 0.5-5 parts；And/or

The aliphatic diamine is 30-60 parts；And/or

The graphene aqueous solution is 5-20 parts；And/or

The end-capping reagent is 0.2-0.3 parts；And/or

The catalyst is 0.02-0.05 parts；And/or

The deionized water is 40-150 parts.

3. static resistant polyamide composite material according to claim 1 or 2, it is characterised in that: the aliphatic dibasic acid Weight fraction ratio with the aromatic acid is 0:100-100:0.

4. static resistant polyamide composite material according to claim 1 or 2, it is characterised in that: the aliphatic dibasic acid Selected from succinic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, azelaic acid, decanedioic acid, heneicosanedioic acid, dodecanedioic acid and One of tridecandioic acid or more than one；And/or

The aromatic acid be selected from one of terephthalic acid (TPA), M-phthalic acid, phthalic acid and naphthalenedicarboxylic acid or More than one；And/or

The aliphatic diamine is selected from butanediamine, pentanediamine, 2 methyl pentamethylenediamine, hexamethylene diamine, nonamethylene diamine, decamethylene diamine, 11 One of alkane diamines, dodecamethylene diamine and tridecane diamine or more than one；And/or

The end-capping reagent be selected from one of benzoic acid, acetic acid, propionic acid, adipic acid or more than one；And/or

The catalyst is selected from sodium phosphate, magnesium phosphate, calcium phosphate, sodium phosphite, phosphorous acid magnesium, Arizona bacilli, zinc phosphite, secondary One of sodium phosphite, ortho phosphorous acid magnesium, Lime Hypophosphate and ortho phosphorous acid zinc or more than one.

5. static resistant polyamide composite material according to claim 4, it is characterised in that: the aliphatic dibasic acid is for oneself One or more of diacid and decanedioic acid；And/or

The aromatic acid is one or more of terephthalic acid (TPA) and M-phthalic acid；And/or

The aliphatic diamine is one or more of hexamethylene diamine and decamethylene diamine；And/or

The end-capping reagent is one or more of acetic acid and adipic acid；And/or

The catalyst is sodium hypophosphite.

6. static resistant polyamide composite material according to claim 1 or 2, it is characterised in that: described to contain sulfonate groups Binary acid be selected from terephthalic acid (TPA) -5- Sulfonic Lithium, terephthalic acid (TPA) -5- sodium sulfonate, terephthalic acid (TPA) -5- potassium sulfonate, to benzene Dioctyl phthalate -5- sulfonic acid rubidium, terephthalic acid (TPA) -5- sulfonic acid caesium, terephthalic acid (TPA) -5- sulfonic acid francium, M-phthalic acid -5- Sulfonic Lithium, 5-sodium sulfo isophthalate, M-phthalic acid -5- potassium sulfonate, M-phthalic acid -5- sulfonic acid rubidium, M-phthalic acid -5- sulfonic acid Caesium, M-phthalic acid -5- sulfonic acid francium, terephthalic acid (TPA) -5- sulfonic acid beryllium, terephthalic acid (TPA) -5- sulfonic acid magnesium, terephthalic acid (TPA) -5- Sulfoacid calcium, terephthalic acid (TPA) -5- sulfonic acid strontium, terephthalic acid (TPA) -5- barium sulfonate, terephthalic acid (TPA) -5- sulfonic acid radium, isophthalic diformazan Acid -5- sulfonic acid beryllium, M-phthalic acid -5- sulfonic acid magnesium, M-phthalic acid -5- sulfoacid calcium, M-phthalic acid -5- sulfonic acid strontium, isophthalic Dioctyl phthalate -5- barium sulfonate, M-phthalic acid -5- sulfonic acid radium, succinic acid sodium sulfonate, adipic acid -2- sodium sulfonate, adipic acid -3- sulphur One of sour sodium, decanedioic acid -2- sodium sulfonate, decanedioic acid -3- sodium sulfonate and decanedioic acid -4- sodium sulfonate or more than one；

Preferably, the binary acid containing sulfonate groups is in 5-sodium sulfo isophthalate and succinic acid sodium sulfonate More than one.

7. static resistant polyamide composite material according to claim 1 or 2, it is characterised in that: the graphene aqueous solution Mass fraction shared by middle graphene is the aqueous solution of 1-10%；And/or

The partial size of the graphene is 0.1-500nm.

8. a kind of preparation method of the static resistant polyamide composite material as described in claim 1 to 7 is any, it is characterised in that: The following steps are included:

(1) binary acid by 20-80 parts of aliphatic/aromatic binary acid, 0.2-10 parts containing sulfonate groups, 20-80 parts of fat Race's diamine, 2-30 part graphene aqueous solution, 0.1-0.4 parts of end-capping reagents, 0.01-0.06 parts of catalyst, 30-160 parts of deionizations Water is added sequentially in autoclave；

(2) it by autoclave vacuum nitrogen gas to replace the air in autoclave, then passes to nitrogen to pressure and reaches 30-50kPa,

(3) autoclave is heated, is warming up to the first temperature, isothermal reaction 1-3 hours；

(4) it is continuously heating to second temperature, pressure is increased to 1-3MPa, and is made by vapor in release autoclave Pressure maintains 1-3MPa；

(5) slowly reach third temperature to temperature within heating 1-3 hours, heat up pressure release after finishing, while keeping temperature-resistant, It by reacting kettle inner pressure pressure release to normal pressure, is escaped up to without tail gas within 0.5-2 hours.

(6) after the reaction was completed, inflated with nitrogen to pressure reaches 0.5-1.0MPa in reaction kettle, and material is finally extruded tie rod pelletizing, Obtain the static resistant polyamide composite material.

9. a kind of preparation method of static resistant polyamide composite material as claimed in claim 8, it is characterised in that: described first Temperature is 80-150 DEG C, and the second temperature is 180-240 DEG C, and the third temperature is 220-340 DEG C.

10. a kind of preparation method of static resistant polyamide composite material as claimed in claim 8, it is characterised in that: described Two temperature are higher than the first temperature, and the third temperature is higher than second temperature.

Technical field

The invention belongs to synthesis of polymer material technical field, it is related to a kind of static resistant polyamide composite material and its preparation Method.

Background technique

Polyamide is commonly called as nylon, refers in macromolecular main chain containing there are many a major class of recurring amide radical group (- CONH-) Polymer.Since nineteen thirty-nine comes out, just it has been more and more widely used.PA6,PA66,PA11,PA12,PA610, The various nylon such as PA612, MXD6 are come out one after another, and now annual yield is more than 270 × 10⁴T occupies important in engineering plastics Status.Polyamide is excellent electrical-insulation polymeric material, and surface resistivity is usually 10¹⁴~10¹⁶Ω, volume resistance Rate is 10¹³~10¹⁴Ω ˙ cm, but only when the surface resistivity of polyamide reaches 10⁸~10¹⁰Ω, volume resistivity reach 10¹¹When Ω ˙ cm, it is just able to satisfy antistatic requirement.Static resistant polyamide is highly important functional polymer material, main to apply In fields such as mining machinery, mine electrical equipment, electronic equipment part, textile machinery parts.

Material can be made to discharge rapidly by the surface conductivity or volume conductance that improve polyamide material prevents electrostatic Aggregation, most common method are the various antistatic agents of addition.Ideal antistatic agent should have antistatic efficiency good and hold Long, heat-resist and polyamide has moderate compatibility.Small organic molecule antistatic agent used now, due to being steamed by surface Hair is influenced to factors such as friction, the washings on moulded products internal migration and surface, and antistatic effect can reduce or even disappear completely It loses, is unable to satisfy the long-term antistatic requirement of product.Permanent antistatic agent is mostly the hydrophily high polymer of a kind of high molecular weight, With lasting antistatic effect, but its additive amount needed it is higher, with the compatibility of polyamide substrate is poor, cost of material compared with Height equally limits such static resistant polyamide composite material so that the mechanical property of product is poor, poor fluidity, price are high Be widely used.

There is the polymerization process for being reported in polyamide that graphene is added, by graphene interconnected, so that material has Preferable conductivity reduces the surface resistivity and volume resistivity of material, reaches the requirement of static resistant polyamide, but nanoscale Graphene surface can be very high, easily reunite, do not propose how rationally to solve graphene in these reports in polyamide preparation Agglomeration traits in the process, so that conductive effect of graphene is had a greatly reduced quality, the additive amount of only increase graphene be can be only achieved Required electric conductivity and antistatic property.However, the graphene production cost of good dispersion is very under existing processing conditions Height, increasing graphene additive amount will definitely increase the production cost of static resistant polyamide composite material, can equally hinder its application It promotes.

Summary of the invention

In view of the deficiencies of the prior art, primary and foremost purpose is to provide a kind of static resistant polyamide composite material to the present invention.

Second object of the present invention is to provide a kind of preparation method of static resistant polyamide composite material.

In order to achieve the above objectives, solution of the invention is:

20-80 parts of aliphatic/aromatic binary acid,

0.2-10 parts of binary acid containing sulfonate groups,

20-80 parts of aliphatic diamine,

2-30 parts of graphene aqueous solution,

0.1-0.4 parts of end-capping reagent,

0.01-0.06 parts of catalyst,

30-160 parts of deionized water.

Preferably, the aliphatic/aromatic binary acid is 30-60 parts；

Preferably, the binary acid containing sulfonate groups is 0.5-5 parts；

Preferably, the aliphatic diamine is 30-60 parts；

Preferably, the graphene aqueous solution is 5-20 parts；

Preferably, the end-capping reagent is 0.2-0.3 parts；

Preferably, the catalyst is 0.02-0.05 parts；

Preferably, the deionized water is 40-150 parts.

The weight fraction ratio of the aliphatic dibasic acid and the aromatic acid is 0:100-100:0.

The aliphatic dibasic acid be selected from succinic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, azelaic acid, decanedioic acid, One of heneicosanedioic acid, dodecanedioic acid and tridecandioic acid or more than one；

The aromatic acid in terephthalic acid (TPA), M-phthalic acid, phthalic acid and naphthalenedicarboxylic acid one Kind or more than one；

The aliphatic diamine be selected from butanediamine, pentanediamine, 2 methyl pentamethylenediamine, hexamethylene diamine, nonamethylene diamine, decamethylene diamine, One of hendecane diamines, dodecamethylene diamine and tridecane diamine or more than one；

The end-capping reagent be selected from one of benzoic acid, acetic acid, propionic acid, adipic acid or more than one；

The catalyst is selected from sodium phosphate, magnesium phosphate, calcium phosphate, sodium phosphite, phosphorous acid magnesium, Arizona bacilli, phosphorous acid One of zinc, sodium hypophosphite, ortho phosphorous acid magnesium, Lime Hypophosphate and ortho phosphorous acid zinc or more than one.

The binary acid containing sulfonate groups be selected from terephthalic acid (TPA) -5- Sulfonic Lithium, terephthalic acid (TPA) -5- sodium sulfonate, Terephthalic acid (TPA) -5- potassium sulfonate, terephthalic acid (TPA) -5- sulfonic acid rubidium, terephthalic acid (TPA) -5- sulfonic acid caesium, terephthalic acid (TPA) -5- sulfonic acid Francium, M-phthalic acid -5- Sulfonic Lithium, 5-sodium sulfo isophthalate, M-phthalic acid -5- potassium sulfonate, M-phthalic acid -5- Sulfonic acid rubidium, M-phthalic acid -5- sulfonic acid caesium, M-phthalic acid -5- sulfonic acid francium, terephthalic acid (TPA) -5- sulfonic acid beryllium, terephthaldehyde Acid -5- sulfonic acid magnesium, terephthalic acid (TPA) -5- sulfoacid calcium, terephthalic acid (TPA) -5- sulfonic acid strontium, terephthalic acid (TPA) -5- barium sulfonate, to benzene Dioctyl phthalate -5- sulfonic acid radium, M-phthalic acid -5- sulfonic acid beryllium, M-phthalic acid -5- sulfonic acid magnesium, M-phthalic acid -5- sulfoacid calcium, M-phthalic acid -5- sulfonic acid strontium, M-phthalic acid -5- barium sulfonate, M-phthalic acid -5- sulfonic acid radium, succinic acid sodium sulfonate, oneself two Acid -2- sodium sulfonate, adipic acid -3- sodium sulfonate, decanedioic acid -2- sodium sulfonate, decanedioic acid -3- sodium sulfonate and decanedioic acid -4- sodium sulfonate One of or more than one；

Mass fraction shared by graphene is 1-10% in the graphene aqueous solution；

The partial size of the graphene is 0.1-500nm.

A kind of preparation method of static resistant polyamide composite material comprising following steps:

(1) binary acid by 20-80 parts of aliphatic/aromatic binary acid, 0.2-10 parts containing sulfonate groups, 20-80 parts Aliphatic diamine, 2-30 part graphene aqueous solution, 0.1-0.4 parts of end-capping reagents, 0.01-0.06 parts of catalyst, 30-160 parts go Ionized water is added sequentially in autoclave；

(2) by autoclave vacuum nitrogen gas to replace the air in autoclave, nitrogen is then passed to pressure Power reaches 30-50kPa,

(3) autoclave is heated, is warming up to the first temperature, isothermal reaction 1-3 hours；

(4) it is continuously heating to second temperature, pressure is increased to 1-3MPa, and is steamed by water in release autoclave Gas makes pressure maintain 1-3MPa；

(5) slowly reach third temperature to temperature within heating 1-3 hours, heat up pressure release after finishing, while keeping temperature not Become, by reacting kettle inner pressure pressure release to normal pressure, is escaped up to without tail gas within 0.5-2 hours.

(6) after the reaction was completed, inflated with nitrogen to pressure reaches 0.5-1.0MPa in reaction kettle, finally cuts material extrusion tie rod Grain, obtains the static resistant polyamide composite material；

Further, the second temperature is higher than the first temperature, and the third temperature is higher than second temperature；

Further, first temperature is 80-150 DEG C, and the second temperature is 180-240 DEG C, and the third temperature is 220-340℃。

By adopting the above scheme, the beneficial effects of the present invention are:

First, the present invention by the polymerization process of polyamide simultaneously graphene aqueous solution and sulfonate groups is added, And the ion of sulfonate and the polar group of graphene surface form stronger attraction such as hydroxyl, carboxyl, so as to effective Improve graphene characteristic easy to reunite, so that nanoscale graphene can be evenly dispersed in polyamide molecule interchain, improves graphite The electrical efficiency of alkene, improves the antistatic property of product, while reducing the additional amount of graphene in process of producing product, reduces life Produce cost；

Second, the present invention by the polymerization process of polyamide simultaneously graphene aqueous solution and sulfonate groups is added, And the conductive energy of sulfonate ion itself, it acts synergistically with the electric conductivity of graphene, it is quiet further to improve resisting for product Electrical property, and sulfonate is compounded with graphene, it, can be into one while significantly improving the antistatic property of product Step reduces the additional amount of graphene, reduces production cost；

Third, the present invention by the polymerization process of polyamide simultaneously graphene aqueous solution and sulfonate groups is added, Sulfonate ion can make nanoscale graphene polyamide molecule interchain is evenly dispersed, compatibility is splendid, therefore will not influence The mechanical property of polyamide compoiste material, mechanical property is substantially suitable with the pure polyamide for being not added with graphene, avoids There are the inorganic fillers such as addition antistatic agent, especially carbon black, so that polyamide compoiste material mechanical property was substantially reduced Problem；

4th, the present invention by the polymerization process of polyamide simultaneously graphene aqueous solution and sulfonate groups is added, Sulfonate ion can make nanoscale graphene evenly dispersed in polyamide molecule interchain, and during product crystallisation by cooling from To the effect of nucleating agent, nucleus, promotion product crystallization are provided for the crystallization of polyamide molecule chain, improves the thermal deformation temperature of product Degree；

5th, the present invention by the polymerization process of polyamide simultaneously graphene aqueous solution and sulfonate groups is added, Sulfonate ion may also function as the effect of lubricant, so as to improve the mobility of polyamide compoiste material, is blended and changes in the later period Property during can greatly increase the contents of the third components such as glass, so as to improve product mechanical property, reduce production cost.

6th, the present invention by the polymerization process of polyamide simultaneously graphene aqueous solution and sulfonate groups is added, Sulfonate ion can make nanoscale graphene evenly dispersed in polyamide molecule interchain, and graphene and sulfonate groups have very Good thermal stability, in the blending and modifying and use process in later period, processing and use environment temperature can also be increased, and improve The flexibility of blending and modifying technique, the application range for expanding product；

7th, the present invention by the polymerization process of polyamide simultaneously graphene aqueous solution and sulfonate groups is added, Sulfonate ion can make nanoscale graphene evenly dispersed in polyamide molecule interchain, can be according to antistatic in practical application It is required that graphene and sulfonate content in flexible modulation product, to meet the requirement of practical application.

Specific embodiment

The present invention provides a kind of static resistant polyamide composite material and preparation methods.

<static resistant polyamide composite material>

A kind of static resistant polyamide composite material, raw materials for production comprise the following components in parts by weight:

20-80 parts of aliphatic/aromatic binary acid,

0.2-10 parts of binary acid containing sulfonate groups,

20-80 parts of aliphatic diamine,

2-30 parts of graphene aqueous solution,

0.1-0.4 parts of end-capping reagent,

0.01-0.06 parts of catalyst,

30-160 parts of deionized water.

Wherein, the aliphatic/aromatic binary acid is preferably 30-60 parts

Aliphatic diamine can be preferably 30-60 parts.

Binary acid containing sulfonate groups can be preferably 0.5-5 parts.

End-capping reagent can be preferably 0.2-0.3 parts.

Catalyst can be preferably 0.02-0.05 parts.

Deionized water can be preferably 40-150 parts.

The weight fraction ratio of aliphatic dibasic acid and the aromatic acid can be between 0:100-100:0.

Graphene aqueous solution can be the aqueous solution that mass fraction shared by graphene is 1-10%.

Aliphatic dibasic acid can be succinic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, azelaic acid, decanedioic acid, ten One or more of one docosandioic acid, dodecanedioic acid and tridecandioic acid.

Aromatic acid can be one of terephthalic acid (TPA), M-phthalic acid, phthalic acid and naphthalenedicarboxylic acid Or more than one.

Aliphatic diamine can be butanediamine, pentanediamine, 2 methyl pentamethylenediamine, hexamethylene diamine, nonamethylene diamine, decamethylene diamine, ten One or more of one alkane diamines, dodecamethylene diamine and tridecane diamine.

End-capping reagent can for one of benzoic acid, acetic acid, propionic acid, adipic acid or more than one.

Catalyst can be sodium phosphate, magnesium phosphate, calcium phosphate, sodium phosphite, phosphorous acid magnesium, Arizona bacilli, zinc phosphite, One of sodium hypophosphite, ortho phosphorous acid magnesium, Lime Hypophosphate and ortho phosphorous acid zinc or more than one.

Binary acid containing sulfonate groups can be terephthalic acid (TPA) -5- Sulfonic Lithium, terephthalic acid (TPA) -5- sodium sulfonate, right Phthalic acid -5- potassium sulfonate, terephthalic acid (TPA) -5- sulfonic acid rubidium, terephthalic acid (TPA) -5- sulfonic acid caesium, terephthalic acid (TPA) -5- sulfonic acid Francium, M-phthalic acid -5- Sulfonic Lithium, 5-sodium sulfo isophthalate, M-phthalic acid -5- potassium sulfonate, M-phthalic acid -5- Sulfonic acid rubidium, M-phthalic acid -5- sulfonic acid caesium, M-phthalic acid -5- sulfonic acid francium, terephthalic acid (TPA) -5- sulfonic acid beryllium, terephthaldehyde Acid -5- sulfonic acid magnesium, terephthalic acid (TPA) -5- sulfoacid calcium, terephthalic acid (TPA) -5- sulfonic acid strontium, terephthalic acid (TPA) -5- barium sulfonate, to benzene Dioctyl phthalate -5- sulfonic acid radium, M-phthalic acid -5- sulfonic acid beryllium, M-phthalic acid -5- sulfonic acid magnesium, M-phthalic acid -5- sulfoacid calcium, M-phthalic acid -5- sulfonic acid strontium, M-phthalic acid -5- barium sulfonate, M-phthalic acid -5- sulfonic acid radium, succinic acid sodium sulfonate, oneself two Acid -2- sodium sulfonate, adipic acid -3- sodium sulfonate, decanedioic acid -2- sodium sulfonate, decanedioic acid -3- sodium sulfonate and decanedioic acid -4- sodium sulfonate One of or more than one.

<preparation method of static resistant polyamide composite material>

A kind of preparation method of static resistant polyamide composite material comprising following steps:

(1) binary acid by 20-80 parts of aliphatic/aromatic binary acid, 0.2-10 parts containing sulfonate groups, 20-80 parts Aliphatic diamine, 2-30 part graphene aqueous solution, 0.1-0.4 parts of end-capping reagents, 0.01-0.06 parts of catalyst, 30-160 parts go Ionized water is added sequentially in autoclave；

(2) by autoclave vacuum nitrogen gas to replace the air in autoclave, nitrogen is then passed to pressure Power reaches 30-50kPa,

(3) autoclave is heated, is warming up to the first temperature, isothermal reaction 1-3 hours；

(4) it is continuously heating to second temperature, pressure is increased to 1-3MPa, and is steamed by water in release autoclave Gas makes pressure maintain 1-3MPa；

(5) slowly reach third temperature DEG C to temperature within heating 1-3 hours, heat up pressure release after finishing, while keeping temperature It is constant, it by reacting kettle inner pressure pressure release to normal pressure, is escaped up to without tail gas within 0.5-2 hours.

(6) after the reaction was completed, inflated with nitrogen to pressure reaches 0.5-1.0MPa in reaction kettle, finally cuts material extrusion tie rod Grain, obtains the static resistant polyamide composite material；

Wherein, first temperature is 80-150 DEG C, and the second temperature is 180-240 DEG C, and the third temperature is 220-340 DEG C, and the second temperature is higher than the first temperature, and the third temperature is higher than second temperature；

In step (2), pressure can be preferably 40kPa.

In step (3), the first temperature is preferably to 110 DEG C.

In step (3), the time of isothermal reaction can be preferably 1.5 hours.

In step (4), second temperature can be preferably to 200-220 DEG C.

In step (4), pressure can be preferably 2MPa.

In step (5), third temperature is preferably 220-290 DEG C.

In step (5), venting duration can be preferably 1 hour.

In step (6), the pressure being filled with after nitrogen can be preferably 0.7MPa.

Below in conjunction with illustrated embodiment and comparative example, the present invention is further illustrated.

Comparative example 1

The preparation method of the static resistant polyamide composite material of this comparative example comprising following steps:

(1), the graphene that parts by weight are 56 parts of adipic acids, 44 parts of hexamethylene diamines, 20 parts of graphene mass fractions are 5% is weighed Aqueous solution, 0.25 part of end-capping reagent acetic acid, 0.03 part of catalyst sodium hypophosphite, 100 parts of deionized waters, and the above component is added Into autoclave；

(2), vacuumize, inflated with nitrogen three times, replace autoclave in air, then pass to nitrogen to pressure and reach 40kPa, so that reaction carries out under inert gas protection always, heating autoclave is warming up to 100 DEG C, isothermal reaction 1.5 Hour；It is continuously heating to 220 DEG C later, pressure is increased to 2MPa, passes through the method for vapor in release reaction kettle at this time It keeps pressure in 2MPa, slowly pressure release after 1.5 hours to 275 DEG C of heating, while keeping temperature-resistant, through 1 hour by reaction kettle Interior pressure pressure release is to normal pressure, until escaping without tail gas.

(3), after the reaction was completed, inflated with nitrogen to pressure reaches 0.7MPa in reaction kettle, and material is finally extruded tie rod pelletizing, Product is obtained, the thermodynamic property and electrical performance testing of products therefrom the results are shown in Table 1.

Comparative example 2

The preparation method of the static resistant polyamide composite material of this comparative example comprising following steps:

(1), weighing parts by weight is 54 parts of adipic acids, 44 parts of hexamethylene diamines, 2 parts of succinic acid sodium sulfonates, 0.25 part of end-capping reagent second Acid, 0.03 part of catalyst sodium hypophosphite, 100 parts of deionized waters, and the above component is added in autoclave；

(2), vacuumize, inflated with nitrogen three times, replace autoclave in air, then pass to nitrogen to pressure and reach 40kPa, so that reaction carries out under inert gas protection always, heating autoclave is warming up to 100 DEG C, isothermal reaction 1.5 Hour；It is continuously heating to 220 DEG C later, pressure is increased to 2MPa, passes through the method for vapor in release reaction kettle at this time It keeps pressure in 2MPa, slowly pressure release after 1.5 hours to 275 DEG C of heating, while keeping temperature-resistant, through 1 hour by reaction kettle Interior pressure pressure release is to normal pressure, until escaping without tail gas.

(3), after the reaction was completed, inflated with nitrogen to pressure reaches 0.7MPa in reaction kettle, and material is finally extruded tie rod pelletizing, Product is obtained, the thermodynamic property and electrical performance testing of products therefrom the results are shown in Table 1.