CN103910997A - Permanent antistatic antibacterial polyamide 6/polypropylene composite material - Google Patents
Permanent antistatic antibacterial polyamide 6/polypropylene composite material Download PDFInfo
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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Abstract
The invention discloses a permanent antistatic antibacterial polyamide 6/polypropylene composite material. The permanent antistatic antibacterial polyamide 6/polypropylene composite material comprises the following components in parts by weight: 100 parts of polyamide 6, 50-100 parts of polypropylene, 20-60 parts of permanent antistatic agent, 0.5-3 parts of antibacterial agent, 10-30 parts of compatilizer, 0.4-1.2 parts of antioxidant and 0.3-0.6 part of lubricant. The permanent antistatic antibacterial polyamide 6/polypropylene composite material disclosed by the invention has the characteristics of permanent antistatic effect, high antibacterial ratio and the like and can be widely applied to the fields such as sanitation, food, daily necessities, medical treatment, electrics, electronics, home appliances, automobiles and national defense.
Description
technical field:
The present invention relates to modifying plastics field, relate in particular to a kind of permanent anti-static, antimicrobial polyamide 6/polypropylene composite material.
background technology:
Polypropylene (be called for short: PP) because it is cheap, excellent performance, source extensively, easily processing, be widely used in the every field such as automobile, household electrical appliances, packing, medical treatment, become modern Application one of plastics the most widely.Polypropylene has that light weight, nontoxic, odorless, chemical stability are good, excellent (generally, its surface resistivity is 10 for electrical property
16~ 10
18Ω), under normal temperature, be insoluble to the advantages such as common solvent, water-absorbent be little; There are a series of shortcomings such as wear resisting property is poor, resistance toheat is poor, toughness is low, barrier properties for gases is poor in polypropylene so, limited its application at some specific area.
(be called for short: PA6) thermomechanical property excellence, good toughness, chemical-resistant are good, (generally, its surface resistivity is 10 to also have good wear resistance, self lubricity and excellent electrical property for polyamide 6
13~ 10
16the advantage such as Ω); So it easily absorbs water, and processing characteristics is poor.In recent years, prepared by polypropylene and polyamide 6 blend to the research of alloy of common occurrence.
Because polypropylene and polyamide 6 all have good electrical insulating property, easily producing accumulation of static electricity with external world's friction or while peeling off, finally cause dust and dirt to be adsorbed in product surface like this, may presence of fire or blast when serious.For fear of this electrostatic phenomenon, must carry out it antistatic modified, to adapt to some specific Application Areas.For macromolecular material, generally prevent and the method for eliminating static mainly contains: (1) adds organic molecule type static inhibitor; (2) prepare alloy with conducting polymer composite blend; (3) add organic macromolecule type static inhibitor; (4) add inorganic conductive material.
Carbon nanotube (Cabon Nanotubes is called for short CNTs), has another name called Baji-tube, is the One-dimensional Quantum material that one has special construction (radial dimension is nanometer scale, and axial dimension is micron dimension, and all seal substantially at pipe two ends).Carbon nanotube is mainly made up of the coaxial pipe of several layers to tens of layers the carbon atom that is hexagonal array.Carbon nanotube has light weight, superelevation mechanical property and good electrical property, be widely used in recent years the enhancing of matrix material, toughness reinforcing and heat conduction, conduction field, its thermal conductivity up to 2800 ~ 4000W/ (m*K) and specific conductivity up to 150 ~ 500S/cm.Be applied in plastic base composite material, can significantly improve heat conduction, conduction and the wear resisting property of plastics.
summary of the invention:
The present invention is directed to the deficiencies in the prior art, a kind of permanent anti-static, antimicrobial polyamide 6/polypropylene composite material are provided.
This permanent anti-static of the present invention, antimicrobial polyamide 6/polypropylene composite material are made up of following components in mass portion:
100 parts of polyamide 6s,
50 ~ 100 parts of polypropylene,
20 ~ 60 parts of permanent anti-static agent,
0.5 ~ 3 part of antiseptic-germicide,
10 ~ 30 parts of compatilizers,
0.4 ~ 1.2 part, oxidation inhibitor,
0.3 ~ 0.6 part of lubricant.
Above-mentioned permanent anti-static agent is the mixture of permanent Polymer Antistatic Agent and permanent inorganic type static inhibitor, and both mass ratioes are 9:1 ~ 19:1.
Above-mentioned antiseptic-germicide is inorganic antiseptic.
Upper polypropylene is more than one in homo-polypropylene (homopolymerization PP), Co-polypropylene (copolymerization PP).
Above-mentioned permanent Polymer Antistatic Agent is polyether block polymeric amide.
Above-mentioned permanent inorganic type static inhibitor is surface treated carbon nanotube.
Described carbon nanotube is the one in Single Walled Carbon Nanotube, multi-walled carbon nano-tubes, double-walled carbon nano-tube.
Described permanent inorganic type static inhibitor is adopted with the following method and is prepared:
1) dry carbon nanotube is placed in to the mixed acid solution of the vitriol oil and concentrated nitric acid, reflux 12-24 hour, takes out and is washed to PH=7, dry; Wherein, the vitriol oil and concentrated nitric acid volume ratio are 2:3, and carbon nanotube and mixed acid solution mass ratio are 1:5;
2) carbon nanotube after step a) washing and drying is placed in to the mixed acid solution of the vitriol oil and concentrated nitric acid, reflux 12-24 hour, takes out and is washed to PH=7, dry; Wherein, the vitriol oil and concentrated nitric acid volume ratio are 2:1, and the carbon nanotube after washing and drying and mixed acid solution mass ratio are 1:4;
3) by step 2) gained carbon nanotube mixes according to mass ratio 1:5 with coupling agent-ethanol solution, and gained slurries are put into ball mill ball milling 1-3 hour, by the vacuum-drying of gained carbon nanotube; In described coupling agent-ethanol solution, coupling agent and dehydrated alcohol mass ratio are 1:8, and adjust pH2 ~ 5; Described coupling agent is that silane coupling agent and titanate coupling agent are composite, and wherein silane coupling agent can be γ-aminopropyl triethoxysilane (KH550), and titanate coupling agent can be sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester (DN-201).
Above-mentioned inorganic antiseptic is silver system and/or zinc series antibacterial agent.
Above-mentioned compatilizer is more than one in polypropylene grafted maleic anhydride (PP-g-MAH), ethylene-methyl acrylate-glyceryl methacrylate terpolymer (E-MA-GMA).
Above-mentioned oxidation inhibitor is selected four [β-(3; 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (antioxidant 1010), three [2; 4-di-tert-butyl-phenyl] phosphorous acid ester (irgasfos 168), N; N'-is two-and three kinds of (3-(3,5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamines (oxidation inhibitor 1098) carry out the composite use of 1:2:1.
Above-mentioned lubricant is that two kinds of ethylene bis stearamide (EBS) and calcium stearates carry out the composite use of 2:1.
The preparation method of above-mentioned permanent anti-static, antimicrobial polyamide 6/polypropylene composite material is as follows: take 100 parts of polyamide 6s, 50 ~ 100 parts of polypropylene, 20 ~ 60 parts of permanent anti-static agent, 0.5 ~ 3 part of antiseptic-germicide, 10 ~ 30 parts of compatilizers, 0.4 ~ 1.2 part of oxidation inhibitor, 0.3 ~ 0.6 part of lubricant and in high-speed mixer, mix 5 minutes, mixing machine rotating speed is 200 revs/min; Then the mixture mixing is added in twin screw extruder melt extrude, cooling
Pelletizing, dress bag, wherein the temperature of forcing machine is followed successively by 180 ℃, 210 ℃, 210 ℃, 220 ℃, 220 ℃, 220 ℃, 220 ℃, 225 ℃ from spout to head.
The present invention uses special method to carry out surface treatment to carbon nanotube, makes it be easier to be scattered in matrix resin material.The present invention combines special carbon nanotube the antistatic effect and the antistatic persistence that use raising plastic base composite material with Polymer Antistatic Agent, and adds therein effective inorganic antiseptic to prepare a kind of permanent anti-static, antimicrobial polyamide 6/polypropylene composite material.
Beneficial effect of the present invention is:
1. the present invention proposes to utilize this mode of the present invention to carry out surface-treated particular form to carbon nanotube first.This processing is conducive to the dispersion of carbon nanotube in plastic substrate, makes antistatic effect remarkable.
2. the present invention is first by Polymer Antistatic Agent and the composite use of inorganic antistatic agent.The effect of both composite uses is better than both independent use antistatic effects, and major cause is that the existence of Polymer Antistatic Agent increases inorganic type static inhibitor dispersion effect.
3. the present invention concentrates on permanent anti-static and antibacterial two effects on plastic base composite material first.The range of application of plastic base composite material is expanded greatly.
embodiment:
below in conjunction with some embodiment and comparative example, the invention will be further described.
The material of using in embodiment and comparative example has:
Single Walled Carbon Nanotube model: CNT100(is without surface treatment) Beijing Deco Dao Jin Science and Technology Ltd.;
Multi-wall carbon nano tube type number: CNT102(is without surface treatment) Beijing Deco Dao Jin Science and Technology Ltd.;
Polyamide 6 model: PA6 M2500 newly understands in Guangzhou U.S.A and reaches;
Co-polypropylene model: BX3800 Korea S SK;
Homo-polypropylene model: T30S China Petrochemical Industry Lanzhou Petrochemical;
Polymer Antistatic Agent model: MV2080 France A Kema;
Inorganic antiseptic model: AGZ330 Japan S.R business Co., Ltd.;
Compatibilizer PP-g-MAH model: 1001 Italian Pulis are bright;
Compatilizer E-MA-GMA model: AX8900 France A Kema;
Antioxidant 1010 model: Irganox1010 Switzerland Ciba;
Oxidation inhibitor 1098 models: Irganox1098 Switzerland Ciba;
Irgasfos 168 model: Irganox168 Switzerland Ciba;
Lubricant model: Chaoyang Chemical Co., Ltd. of EBS Indonesia;
Lubricant model: the friend of calcium stearate (premium grads) Gaomi City of Shandong Province and auxiliary agent company limited;
Coupling agent model: KH550 Nanjing Dao Ning Chemical Co., Ltd.;
Coupling agent model: DN-201 Nanjing Dao Ning Chemical Co., Ltd.;
Vitriol oil model: mass concentration 98% Shandong Zibo vitriol works;
Concentrated nitric acid model: mass concentration 65% Dongguan City Sheng Neng Chemical Co., Ltd..
In all embodiment and comparative example, if no special instructions, described umber is mass parts below, surface resistivity test execution GB/T 1410, and test condition for testing under 23 ℃, humidity 50% condition; Anti-microbial property test execution QB/T 2591, test condition is tested for placing to cultivate after 24 hours under 23 ℃, humidity 50% condition.
embodiment 1
Step 1: carbon nano tube surface processing;
Take the addition of C NT100 type Single Walled Carbon Nanotube, be placed in 120 ℃ of baking ovens, dry 6 hours is 1:5 mixing match, reflux under agitator effect by dry carbon nanotube and nitration mixture (vitriol oil: concentrated nitric acid volume ratio is that 2:3 mixes) in mass ratio, treatment temp is 150 ℃, treatment time is 24 hours, takes out handled thing, is repeatedly washed with distilled water to PH=7, put into 120 ℃ of baking ovens, dry 10 hours.Then be 1:4 mixing match in mass ratio by dry carbon nanotube and nitration mixture (vitriol oil: concentrated nitric acid volume ratio is that 2:1 mixes), reflux under agitator effect, treatment temp is 150 ℃, treatment time is 24 hours, take out handled thing, repeatedly be washed with distilled water to PH=7, put into 120 ℃ of baking ovens, dry 12 hours.
By above-mentioned dried carbon nanotube and coupling agent-ethanol solution (coupling agent: dehydrated alcohol mass ratio is 1:8, and dripping hydrochloric acid soln, to adjust pH value be between 2 ~ 5.) be that 1:5 mixes according to mass ratio, the slurries of gained are put into ball mill and are carried out ball milling 2 hours, and 400 revs/min of rotating speeds are finally placed in obtained carbon nanotube 120 ℃ of baking ovens of vacuum, dry 10 hours.Stand-by.
Note: coupling agent is silane coupling agent, the composite use of titanate coupling agent, wherein silane coupling agent is that γ-aminopropyl triethoxysilane (KH550) and titanate coupling agent are sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester (DN-201), carries out composite use according to mass ratio 1:1.
Step 2: permanent anti-static, the preparation of antimicrobial polyamide 6/polypropylene composite material;
Take carbon nanotube, 0.5 part of antiseptic-germicide AGZ330,1001,0.1 part of antioxidant 1010 of 10 parts of compatilizers, 1098,0.2 part of irgasfos 168 of 0.1 part of oxidation inhibitor, 0.2 part of Lubricate EBS, 0.1 part of calcium stearate prepared by 100 parts of PA6 M2500,50 parts of polypropylene BX3800,19 parts of MV2080,1 part of step 1 and in high-speed mixer, mix 5 minutes, mixing machine rotating speed is 200 revs/min; Then the mixture mixing is added in twin screw extruder melt extrude, cooling and dicing, dress bag, wherein the temperature of forcing machine is followed successively by 180 ℃, 210 ℃, 210 ℃, 220 ℃, 220 ℃, 220 ℃, 220 ℃, 225 ℃ from spout to head.Performance is as table-1.
comparative example 1
Step 1: carbon nano tube surface processing;
Take the addition of C NT100 type Single Walled Carbon Nanotube, be placed in 120 ℃ of baking ovens, dry 6 hours is 1:5 mixing match, reflux under agitator effect by dry carbon nanotube and nitration mixture (vitriol oil: concentrated nitric acid volume ratio is that 2:3 mixes) in mass ratio, treatment temp is 150 ℃, treatment time is 24 hours, takes out handled thing, is repeatedly washed with distilled water to PH=7, put into 120 ℃ of baking ovens, dry 10 hours.Then be 1:4 mixing match in mass ratio by dry carbon nanotube and nitration mixture (vitriol oil: concentrated nitric acid volume ratio is that 2:1 mixes), reflux under agitator effect, treatment temp is 150 ℃, treatment time is 24 hours, take out handled thing, repeatedly be washed with distilled water to PH=7, put into 120 ℃ of baking ovens, dry 12 hours.
By above-mentioned dried carbon nanotube and coupling agent-ethanol solution (coupling agent: dehydrated alcohol mass ratio is 1:8, and dripping hydrochloric acid soln, to adjust pH value be between 2 ~ 5.) be that 1:5 mixes according to mass ratio, the slurries of gained are put into ball mill and are carried out ball milling 2 hours, and 400 revs/min of rotating speeds are finally placed in obtained carbon nanotube 120 ℃ of baking ovens of vacuum, dry 10 hours.Stand-by.
Note: coupling agent is silane coupling agent, the composite use of titanate coupling agent, wherein silane coupling agent is that γ-aminopropyl triethoxysilane (KH550) and titanate coupling agent are sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester (DN-201), carries out composite use according to 1:1.
Step 2: permanent anti-static, the preparation of antimicrobial polyamide 6/polypropylene composite material;
Take carbon nanotube, 1001,0.1 part of antioxidant 1010 of 10 parts of compatilizers, 1098,0.2 part of irgasfos 168 of 0.1 part of oxidation inhibitor, 0.2 part of Lubricate EBS, 0.1 part of calcium stearate prepared by 100 parts of PA6 M2500,50 parts of polypropylene BX3800,19 parts of MV2080,1 part of step 1 and in high-speed mixer, mix 5 minutes, mixing machine rotating speed is 200 revs/min; Then the mixture mixing is added in twin screw extruder melt extrude, cooling
Pelletizing, dress bag, wherein the temperature of forcing machine is followed successively by 180 ℃, 210 ℃, 210 ℃, 220 ℃, 220 ℃, 220 ℃, 220 ℃, 225 ℃ from spout to head.Performance is as table-1.
comparative example 2
Step 1: permanent anti-static, the preparation of antimicrobial polyamide 6/polypropylene composite material;
Take 100 parts of PA6 M2500,50 parts of polypropylene BX3800,20 parts of MV2080,0.5 part of antiseptic-germicide AGZ330,1001,0.1 part of antioxidant 1010 of 10 parts of compatilizers, 1098,0.2 part of irgasfos 168 of 0.1 part of oxidation inhibitor, 0.2 part of Lubricate EBS, 0.1 part of calcium stearate mix 5 minutes in high-speed mixer, mixing machine rotating speed is 200 revs/min; Then the mixture mixing is added in twin screw extruder melt extrude, cooling
Pelletizing, dress bag, wherein the temperature of forcing machine is followed successively by 180 ℃, 210 ℃, 210 ℃, 220 ℃, 220 ℃, 220 ℃, 220 ℃, 225 ℃ from spout to head.Performance is as table-1.
comparative example 3
Step 1: carbon nano tube surface processing;
Take the addition of C NT100 type Single Walled Carbon Nanotube, be placed in 120 ℃ of baking ovens, dry 6 hours is 1:5 mixing match, reflux under agitator effect by dry carbon nanotube and nitration mixture (vitriol oil: concentrated nitric acid volume ratio is that 2:3 mixes) in mass ratio, treatment temp is 150 ℃, treatment time is 24 hours, takes out handled thing, is repeatedly washed with distilled water to PH=7, put into 120 ℃ of baking ovens, dry 10 hours.Then be 1:4 mixing match in mass ratio by dry carbon nanotube and nitration mixture (vitriol oil: concentrated nitric acid volume ratio is that 2:1 mixes), reflux under agitator effect, treatment temp is 150 ℃, treatment time is 24 hours, take out handled thing, repeatedly be washed with distilled water to PH=7, put into 120 ℃ of baking ovens, dry 12 hours.
By above-mentioned dried carbon nanotube and coupling agent-ethanol solution (coupling agent: dehydrated alcohol mass ratio is 1:8, and dripping hydrochloric acid soln, to adjust pH value be between 2 ~ 5.) be that 1:5 mixes according to mass ratio, the slurries of gained are put into ball mill and are carried out ball milling 2 hours, and 400 revs/min of rotating speeds are finally placed in obtained carbon nanotube 120 ℃ of baking ovens of vacuum, dry 10 hours.Stand-by.
Note: coupling agent is silane coupling agent, the composite use of titanate coupling agent, wherein silane coupling agent is that γ-aminopropyl triethoxysilane (KH550) and titanate coupling agent are sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester (DN-201), carries out composite use according to 1:1.
Step 2: permanent anti-static, the preparation of antimicrobial polyamide 6/polypropylene composite material;
Take carbon nanotube, 0.5 part of antiseptic-germicide AGZ330,1001,0.1 part of antioxidant 1010 of 10 parts of compatilizers, 1098,0.2 part of irgasfos 168 of 0.1 part of oxidation inhibitor, 0.2 part of Lubricate EBS, 0.1 part of calcium stearate prepared by 100 parts of PA6 M2500,50 parts of polypropylene BX3800,20 parts of step 1 and in high-speed mixer, mix 5 minutes, mixing machine rotating speed is 200 revs/min; Then the mixture mixing is added in twin screw extruder melt extrude, cooling and dicing, dress bag, wherein the temperature of forcing machine is followed successively by 180 ℃, 210 ℃, 210 ℃, 220 ℃, 220 ℃, 220 ℃, 220 ℃, 225 ℃ from spout to head.Performance is as table-1.
Table-1 embodiment 1 and comparative example 1 ~ 3 performance
From above embodiment 1 and comparative example 1 ~ 3 relatively can obviously find out, matrix material of the present invention has preferably antistatic and antibacterial effect.Comparative example 1 and comparative example 2,3 can find out, Polymer Antistatic Agent and the composite result of use of inorganic type static inhibitor are better than independent use, and in comparative example 3, carbon nanotube usage quantity is excessive, causes reuniting, and makes antistatic effect not as good as embodiment 1.
embodiment 2
Step 1: carbon nano tube surface processing;
Take the addition of C NT102 type multi-walled carbon nano-tubes, be placed in 120 ℃ of baking ovens, dry 6 hours is 1:5 mixing match, reflux under agitator effect by dry carbon nanotube and nitration mixture (vitriol oil: concentrated nitric acid volume ratio is that 2:3 mixes) in mass ratio, treatment temp is 150 ℃, treatment time is 24 hours, takes out handled thing, is repeatedly washed with distilled water to PH=7, put into 120 ℃ of baking ovens, dry 10 hours.Then be 1:4 mixing match in mass ratio by dry carbon nanotube and nitration mixture (vitriol oil: concentrated nitric acid volume ratio is that 2:1 mixes), reflux under agitator effect, treatment temp is 150 ℃, treatment time is 24 hours, take out handled thing, repeatedly be washed with distilled water to PH=7, put into 120 ℃ of baking ovens, dry 12 hours.
By above-mentioned dried carbon nanotube and coupling agent-ethanol solution (coupling agent: dehydrated alcohol mass ratio is 1:8, and dripping hydrochloric acid soln, to adjust pH value be between 2 ~ 5.) be that 1:5 mixes according to mass ratio, the slurries of gained are put into ball mill and are carried out ball milling 2 hours, and 400 revs/min of rotating speeds are finally placed in obtained carbon nanotube 120 ℃ of baking ovens of vacuum, dry 10 hours.Stand-by.
Note: coupling agent is silane coupling agent, the composite use of titanate coupling agent, wherein silane coupling agent is that γ-aminopropyl triethoxysilane (KH550) and titanate coupling agent are sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester (DN-201), carries out composite use according to 1:1.
Step 2: permanent anti-static, the preparation of antimicrobial polyamide 6/polypropylene composite material;
Take carbon nanotube, 3 parts of antiseptic-germicide AGZ330,30 parts of compatilizer AX8900,0.3 part of antioxidant 1010,1098,0.6 part of irgasfos 168 of 0.3 part of oxidation inhibitor, 0.4 part of Lubricate EBS, 0.2 part of calcium stearate prepared by 100 parts of PA6 M2500,100 parts of polypropylene T30S, 54 parts of MV2080,6 parts of step 1 and in high-speed mixer, mix 5 minutes, mixing machine rotating speed is 200 revs/min; Then the mixture mixing is added in twin screw extruder melt extrude, cooling and dicing, dress bag, wherein the temperature of forcing machine is followed successively by 180 ℃, 210 ℃, 210 ℃, 220 ℃, 220 ℃, 220 ℃, 220 ℃, 225 ℃ from spout to head.Performance is as table-2.
comparative example 4
Step 1: carbon nano tube surface processing;
Take the addition of C NT102 type multi-walled carbon nano-tubes, be placed in 120 ℃ of baking ovens, dry 6 hours is 1:5 mixing match, reflux under agitator effect by dry carbon nanotube and nitration mixture (vitriol oil: concentrated nitric acid volume ratio is that 2:3 mixes) in mass ratio, treatment temp is 150 ℃, treatment time is 24 hours, takes out handled thing, is repeatedly washed with distilled water to PH=7, put into 120 ℃ of baking ovens, dry 10 hours.
By above-mentioned dried carbon nanotube and coupling agent-ethanol solution (coupling agent: dehydrated alcohol mass ratio is 1:8, and dripping hydrochloric acid soln, to adjust pH value be between 2 ~ 5.) be that 1:5 mixes according to mass ratio, the slurries of gained are put into ball mill and are carried out ball milling 2 hours, and 400 revs/min of rotating speeds are finally placed in obtained carbon nanotube 120 ℃ of baking ovens of vacuum, dry 10 hours.Stand-by.
Note: coupling agent is silane coupling agent, the composite use of titanate coupling agent, wherein silane coupling agent is that γ-aminopropyl triethoxysilane (KH550) and titanate coupling agent are sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester (DN-201), carries out composite use according to 1:1.
Step 2: permanent anti-static, the preparation of antimicrobial polyamide 6/polypropylene composite material;
Take carbon nanotube, 3 parts of antiseptic-germicide AGZ330,30 parts of compatilizer AX8900,0.3 part of antioxidant 1010,1098,0.6 part of irgasfos 168 of 0.3 part of oxidation inhibitor, 0.4 part of Lubricate EBS, 0.2 part of calcium stearate prepared by 100 parts of PA6 M2500,100 parts of polypropylene T30S, 54 parts of MV2080,6 parts of step 1 and in high-speed mixer, mix 5 minutes, mixing machine rotating speed is 200 revs/min; Then the mixture mixing is added in twin screw extruder melt extrude, cooling and dicing, dress bag, wherein the temperature of forcing machine is followed successively by 180 ℃, 210 ℃, 210 ℃, 220 ℃, 220 ℃, 220 ℃, 220 ℃, 225 ℃ from spout to head.Performance is as table-2.
embodiment 3
Step 1: carbon nano tube surface processing;
Take the addition of C NT102 type multi-walled carbon nano-tubes, be placed in 120 ℃ of baking ovens, dry 6 hours is 1:5 mixing match, reflux under agitator effect by dry carbon nanotube and nitration mixture (vitriol oil: concentrated nitric acid volume ratio is that 2:3 mixes) in mass ratio, treatment temp is 150 ℃, treatment time is 22 hours, takes out handled thing, is repeatedly washed with distilled water to PH=7, put into 120 ℃ of baking ovens, dry 10 hours.Then be 1:4 mixing match in mass ratio by dry carbon nanotube and nitration mixture (vitriol oil: concentrated nitric acid volume ratio is that 2:1 mixes), reflux under agitator effect, treatment temp is 150 ℃, treatment time is 22 hours, take out handled thing, repeatedly be washed with distilled water to PH=7, put into 120 ℃ of baking ovens, dry 12 hours.
By above-mentioned dried carbon nanotube and coupling agent-ethanol solution (coupling agent: dehydrated alcohol mass ratio is 1:8, and dripping hydrochloric acid soln, to adjust pH value be between 2 ~ 5.) be that 1:5 mixes according to mass ratio, the slurries of gained are put into ball mill and are carried out ball milling 2 hours, and 400 revs/min of rotating speeds are finally placed in obtained carbon nanotube 120 ℃ of baking ovens of vacuum, dry 10 hours.Stand-by.
Note: coupling agent is silane coupling agent, the composite use of titanate coupling agent, wherein silane coupling agent is that γ-aminopropyl triethoxysilane (KH550) and titanate coupling agent are sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester (DN-201), carries out composite use according to 1:1.
Step 2: permanent anti-static, the preparation of antimicrobial polyamide 6/polypropylene composite material;
Take carbon nanotube, 1 part of antiseptic-germicide AGZ330,10 parts of compatilizer AX8900,1001,0.12 part of antioxidant 1010 of 10 parts of compatilizers, 1098,0.24 part of irgasfos 168 of 0.12 part of oxidation inhibitor, 0.24 part of Lubricate EBS, 0.12 part of calcium stearate prepared by 100 parts of PA6 M2500,50 parts of polypropylene T30S, 30 parts of polypropylene BX3800,24 parts of MV2080,2 parts of step 1 and in high-speed mixer, mix 5 minutes, mixing machine rotating speed is 200 revs/min; Then the mixture mixing is added in twin screw extruder melt extrude, cooling and dicing, dress bag, wherein the temperature of forcing machine is followed successively by 180 ℃, 210 ℃, 210 ℃, 220 ℃, 220 ℃, 220 ℃, 220 ℃, 225 ℃ from spout to head.Performance is as table-2.
embodiment 4
Step 1: carbon nano tube surface processing;
Take the addition of C NT102 type multi-walled carbon nano-tubes, be placed in 120 ℃ of baking ovens, dry 6 hours is 1:5 mixing match, reflux under agitator effect by dry carbon nanotube and nitration mixture (vitriol oil: concentrated nitric acid volume ratio is that 2:3 mixes) in mass ratio, treatment temp is 150 ℃, treatment time is 18 hours, takes out handled thing, is repeatedly washed with distilled water to PH=7, put into 120 ℃ of baking ovens, dry 10 hours.Then be 1:4 mixing match in mass ratio by dry carbon nanotube and nitration mixture (vitriol oil: concentrated nitric acid volume ratio is that 2:1 mixes), reflux under agitator effect, treatment temp is 150 ℃, treatment time is 18 hours, take out handled thing, repeatedly be washed with distilled water to PH=7, put into 120 ℃ of baking ovens, dry 12 hours.
By above-mentioned dried carbon nanotube and coupling agent-ethanol solution (coupling agent: dehydrated alcohol mass ratio is 1:8, and dripping hydrochloric acid soln, to adjust pH value be between 2 ~ 5.) be that 1:5 mixes according to mass ratio, the slurries of gained are put into ball mill and are carried out ball milling 2 hours, and 400 revs/min of rotating speeds are finally placed in obtained carbon nanotube 120 ℃ of baking ovens of vacuum, dry 10 hours.Stand-by.
Note: coupling agent is silane coupling agent, the composite use of titanate coupling agent, wherein silane coupling agent is that γ-aminopropyl triethoxysilane (KH550) and titanate coupling agent are sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester (DN-201), carries out composite use according to 1:1.
Step 2: permanent anti-static, the preparation of antimicrobial polyamide 6/polypropylene composite material;
Take carbon nanotube, 1.8 parts of antiseptic-germicide AGZ330,8 parts of compatilizer AX8900,1001,0.12 part of antioxidant 1010 of 15 parts of compatilizers, 1098,0.24 part of irgasfos 168 of 0.12 part of oxidation inhibitor, 0.24 part of Lubricate EBS, 0.12 part of calcium stearate prepared by 100 parts of PA6 M2500,50 parts of polypropylene T30S, 50 parts of polypropylene BX3800,48 parts of MV2080,4 parts of step 1 and in high-speed mixer, mix 5 minutes, mixing machine rotating speed is 200 revs/min; Then the mixture mixing is added in twin screw extruder melt extrude, cooling and dicing, dress bag, wherein the temperature of forcing machine is followed successively by 180 ℃, 210 ℃, 210 ℃, 220 ℃, 220 ℃, 220 ℃, 220 ℃, 225 ℃ from spout to head.Performance is as table-2.
embodiment 5
Step 1: carbon nano tube surface processing;
Take the addition of C NT100 type Single Walled Carbon Nanotube, be placed in 120 ℃ of baking ovens, dry 6 hours is 1:5 mixing match, reflux under agitator effect by dry carbon nanotube and nitration mixture (vitriol oil: concentrated nitric acid volume ratio is that 2:3 mixes) in mass ratio, treatment temp is 150 ℃, treatment time is 12 hours, takes out handled thing, is repeatedly washed with distilled water to PH=7, put into 120 ℃ of baking ovens, dry 10 hours.Then be 1:4 mixing match in mass ratio by dry carbon nanotube and nitration mixture (vitriol oil: concentrated nitric acid volume ratio is that 2:1 mixes), reflux under agitator effect, treatment temp is 150 ℃, treatment time is 12 hours, take out handled thing, repeatedly be washed with distilled water to PH=7, put into 120 ℃ of baking ovens, dry 12 hours.
By above-mentioned dried carbon nanotube and coupling agent-ethanol solution (coupling agent: dehydrated alcohol mass ratio is 1:8, and dripping hydrochloric acid soln, to adjust pH value be between 2 ~ 5.) be that 1:5 mixes according to mass ratio, the slurries of gained are put into ball mill and are carried out ball milling 2 hours, and 400 revs/min of rotating speeds are finally placed in obtained carbon nanotube 120 ℃ of baking ovens of vacuum, dry 10 hours.Stand-by.
Note: coupling agent is silane coupling agent, the composite use of titanate coupling agent, wherein silane coupling agent is that γ-aminopropyl triethoxysilane (KH550) and titanate coupling agent are sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester (DN-201), carries out composite use according to 1:1.
Step 2: permanent anti-static, the preparation of antimicrobial polyamide 6/polypropylene composite material;
Take carbon nanotube, 2.5 parts of antiseptic-germicide AGZ330,10 parts of compatilizer AX8900,1001,0.22 part of antioxidant 1010 of 15 parts of compatilizers, 1098,0.44 part of irgasfos 168 of 0.22 part of oxidation inhibitor, 0.34 part of Lubricate EBS, 0.17 part of calcium stearate prepared by 100 parts of PA6 M2500,90 parts of polypropylene T30S, 45 parts of MV2080,3 parts of step 1 and in high-speed mixer, mix 5 minutes, mixing machine rotating speed is 200 revs/min; Then the mixture mixing is added in twin screw extruder melt extrude, cooling and dicing, dress bag, wherein the temperature of forcing machine is followed successively by 180 ℃, 210 ℃, 210 ℃, 220 ℃, 220 ℃, 220 ℃, 220 ℃, 225 ℃ from spout to head.Performance is as table-2.
Table-2 embodiment 2 ~ 5 and comparative example 4 performances
Can find out from above embodiment 2 ~ 5, permanent anti-static prepared by the present invention, the antistatic effect of antimicrobial polyamide 6/polypropylene composite material are remarkable, antibacterial effect excellence.From embodiment 2, can obviously find out, composite material surface resistivity is 10
5the Ω order of magnitude, antibacterium rate is up to more than 99.9%, and antifungal grade is 0 grade of highest ranking.Can find out from embodiments of the invention 2 and comparative example 4, nitration mixture carries out primary treatment and carries out twice processing carbon nanotube, and the effect of its twice processing is more effective than primary treatment.Can find out from above embodiment 3-5, the present invention adds appropriate permanent anti-static agent and appropriate antiseptic-germicide, can reach good antistatic effect and antibacterial effect.
This permanent anti-static of the present invention, antimicrobial polyamide 6/polypropylene composite material, have permanent anti-static effect, antibiotic rate high, can be widely used in defending the fields such as food, daily necessities, medical treatment, electric, household electrical appliances, automobile, national defence.
Claims (10)
1. permanent anti-static, antimicrobial polyamide 6/polypropylene composite material, it is made up of following components in mass portion:
100 parts of polyamide 6s,
50 ~ 100 parts of polypropylene,
20 ~ 60 parts of permanent anti-static agent,
0.5 ~ 3 part of antiseptic-germicide,
10 ~ 30 parts of compatilizers,
0.4 ~ 1.2 part, oxidation inhibitor,
0.3 ~ 0.6 part of lubricant;
Above-mentioned permanent anti-static agent is the permanent Polymer Antistatic Agent of mass ratio 9:1 ~ 19:1 and the mixture of permanent inorganic type static inhibitor; Above-mentioned antiseptic-germicide is inorganic antiseptic.
2. a kind of permanent anti-static, antimicrobial polyamide 6/polypropylene composite material as claimed in claim 1, is characterized in that, described polypropylene is more than one in homo-polypropylene, Co-polypropylene.
3. a kind of permanent anti-static, antimicrobial polyamide 6/polypropylene composite material as claimed in claim 1, is characterized in that, described permanent Polymer Antistatic Agent is polyether block polymeric amide.
4. a kind of permanent anti-static, antimicrobial polyamide 6/polypropylene composite material as claimed in claim 1, is characterized in that, described permanent inorganic type static inhibitor is surface treated carbon nanotube.
5. a kind of permanent anti-static, antimicrobial polyamide 6/polypropylene composite material as claimed in claim 4, is characterized in that, described carbon nanotube is the one in Single Walled Carbon Nanotube, multi-walled carbon nano-tubes, double-walled carbon nano-tube.
6. a kind of permanent anti-static, antimicrobial polyamide 6/polypropylene composite material as claimed in claim 4, is characterized in that, described permanent inorganic type static inhibitor is adopted with the following method and prepared:
1) dry carbon nanotube is placed in to the mixed acid solution of the vitriol oil and concentrated nitric acid, reflux 12-24 hour, takes out and is washed to PH=7, dry; Wherein, the vitriol oil and concentrated nitric acid volume ratio are 2:3, and carbon nanotube and mixed acid solution mass ratio are 1:5;
2) carbon nanotube after step a) washing and drying is placed in to the mixed acid solution of the vitriol oil and concentrated nitric acid, reflux 12-24 hour, takes out and is washed to PH=7, dry; Wherein, the vitriol oil and concentrated nitric acid volume ratio are 2:1, and the carbon nanotube after washing and drying and mixed acid solution mass ratio are 1:4;
3) by step 2) gained carbon nanotube mixes according to mass ratio 1:5 with coupling agent-ethanol solution, and gained slurries are put into ball mill ball milling 1-3 hour, by the vacuum-drying of gained carbon nanotube; In described coupling agent-ethanol solution, coupling agent and dehydrated alcohol mass ratio are 1:8, and adjust pH2 ~ 5; Described coupling agent is that silane coupling agent and titanate coupling agent are composite.
7. a kind of permanent anti-static, antimicrobial polyamide 6/polypropylene composite material as claimed in claim 1, is characterized in that, described inorganic antiseptic is silver system and/or zinc series antibacterial agent.
8. a kind of permanent anti-static, antimicrobial polyamide 6/polypropylene composite material as claimed in claim 1, it is characterized in that, described compatilizer is more than one in polypropylene grafted maleic anhydride, ethylene-methyl acrylate-glyceryl methacrylate terpolymer.
9. a kind of permanent anti-static, antimicrobial polyamide 6/polypropylene composite material as claimed in claim 1; it is characterized in that; described oxidation inhibitor is selected four [β-(3; 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, three [2; 4-di-tert-butyl-phenyl] phosphorous acid ester, N; N'-pair-(3-(3,5-di-tert-butyl-hydroxy phenyl) propionyl) three kinds of hexanediamines are composite.
10. a kind of permanent anti-static, antimicrobial polyamide 6/polypropylene composite material as claimed in claim 1, is characterized in that, described lubricant is that ethylene bis stearamide and two kinds of calcium stearates are composite.
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