CN109265991A - Flame-retardant conductive nylon composite materials and preparation method thereof - Google Patents
Flame-retardant conductive nylon composite materials and preparation method thereof Download PDFInfo
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- CN109265991A CN109265991A CN201811076121.9A CN201811076121A CN109265991A CN 109265991 A CN109265991 A CN 109265991A CN 201811076121 A CN201811076121 A CN 201811076121A CN 109265991 A CN109265991 A CN 109265991A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2244—Oxides; Hydroxides of metals of zirconium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2251—Oxides; Hydroxides of metals of chromium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention proposes a kind of flame-retardant conductive nylon composite materials and preparation method thereof, including following raw material: nylon 610 resin, nylon 11, denatured conductive mica powder, aramid fiber, chromium oxide, zirconium oxide, fire retardant, toughener, compatilizer and antioxidant；Denatured conductive mica powder stone is mainly prepared by conductive mica powder, aluminium borate whisker, conductive black, lube base oil and silane coupling agent.Preparation method are as follows: 1) first chromium oxide, zirconium oxide, denatured conductive mica powder, nylon 610 resin, nylon 11 are uniformly mixed with toughener, prepare master batch with double screw extruder；2) master batch that step 1) obtains is mixed with aramid fiber, fire retardant, antioxidant, compatilizer, through melting extrusion in double screw extruder.The nylon material has excellent electric conductivity and mechanical property.
Description
Technical field
The invention belongs to technical field of polymer materials, and in particular to a kind of flame-retardant conductive nylon composite materials and its preparation
Method.
Background technique
Fypro is commonly called as nylon, and purposes is very extensive, and auto industry is usually used in manufacturing auto parts and components such as instrument
Plate, vehicle-body outer panel, inner trim panels, steering wheel, soundproof plate, door lock, bumper, ventilation duct etc., household electric appliances are usually used in manufacturing such as
Refrigerator, television set, washing machine, vacuum cleaner, food mixer, shell of telephone set etc. are common in architectural decoration
In manufacture such as sanitary apparatus, swimming pool lining, tubing and pipe fitting, after being in addition also used to manufacture safety cap, motorcycle plate washer, shoes
With, daily necessities and the nameplate, ornament such as snowfield sporting goods, toy, clock, casing of loudspeaker box, suitcase, button, minaudiere
Equal advertising matters.
Although Fypro is widely used, due to the characteristic of Fypro molecular structure performance itself, so that poly-
Nylon is insufficient in terms of electric conductivity.Nylon resin has very high sheet resistance, in use since friction is easy to
Surface stored charge causes static discharge, generates electric spark and causes fire.The method that people usually pass through addition conductive filler
Improve the electrical property and heating conduction of polymer, still, to assign nylon resin ideal electric conductivity and heating conduction needs
A large amount of conductive filler is filled, will lead to the moulding processability of composite material and the sharp fall of mechanical property.
Summary of the invention
The present invention proposes that a kind of flame-retardant conductive nylon composite materials, the nylon material have excellent electric conductivity and mechanical property
Energy.
The technical scheme of the present invention is realized as follows:
A kind of flame-retardant conductive nylon composite materials, according to the number of parts by weight, including following raw material:
65~75 parts of nylon 610 resin, 6~12 parts of nylon 11,10~20 parts of denatured conductive mica powder, aramid fiber 2~5
Part, 1~3 part of chromium oxide, 2~4 parts of zirconium oxide, 2~4 parts of fire retardant, 3~8 parts of toughener, 0.4~1.2 part of compatilizer and antioxygen
0.2~0.8 part of agent；The denatured conductive mica powder stone is mainly by conductive mica powder, aluminium borate whisker, conductive black, lubrication
Oil base oil and silane coupling agent are prepared.
Preferably, the denatured conductive mica powder stone preparation method the following steps are included:
1) 40~50 parts of conductive mica powder, 5~10 parts of aluminium borate whisker, conductive black according to the number of parts by weight, are weighed
20~30 parts, 0.4~1.2 part of lube base oil and 0.6~2.4 part of silane coupling agent are spare；
2) by conductive mica powder and aluminium borate whisker carried out in 900~1300 DEG C of vacuum drying ovens after mixing roasting 3~
6h after being cooled to room temperature product of roasting, disperses product of roasting with chitosan aqueous solution, and filtering carries out filtrate
Drying；
3) by filtrate, conductive black, silane coupling agent and the lube base oil after step 2) drying at 75~85 DEG C
Under the conditions of be stirred to react 30~60min.
Preferably, the silane coupling agent is aminopropyl trimethoxysilane or isopro-pyltriethoxysilane.
Preferably, the toughener is selected from maleic anhydride grafted ethene-octene copolymer, glycidyl methacrylate
At least one of grafted ethene-octene copolymer.
Preferably, the compatilizer is selected from for styrene-maleic anhydride copolymer, maleic anhydride grafted polyphenylene ether
At least one.
Preferably, the fire retardant is selected from decabromodiphenylethane or triphenyl phosphate.
Preferably, the antioxidant is three [2,4 di-tert-butyl-phenyl] phosphite esters.
It is a further object to provide a kind of preparation methods of flame-retardant conductive nylon composite materials, including following step
It is rapid:
1) first chromium oxide, zirconium oxide, denatured conductive mica powder, nylon 610 resin, nylon 11 are mixed with toughener
It is even, master batch is prepared with double screw extruder；
2) master batch that step 1) obtains is mixed with aramid fiber, fire retardant, antioxidant, compatilizer, is squeezed through twin-screw
Melting extrusion in machine out.
The invention has the advantages that:
Flame-retardant conductive nylon composite materials of the invention using mainly by mainly by conductive mica powder, aluminium borate whisker, lead
The denatured conductive mica powder that electric carbon black, lube base oil and silane coupling agent are prepared is acted on aramid fiber, so that fragrant
Synthetic fibre fiber can be more uniformly dispersed in nylon, and chromium oxide and zirconium oxide also can be more uniformly dispersed in nylon, be mentioned
The high electron mobility of modified oxidized chromium and zirconium oxide, so that the nylon material not add traditional metal additionally
Powder, graphite and conductive black can have good electric conductivity.
The tensile strength of flame-retardant conductive nylon composite materials polymer composite of the invention is greater than 130MPa, and bending is strong
Degree is greater than 200MPa, and Izod notched impact strength is greater than 20j/m2, and there is the excellent electrostatic efficiency that disappears.
Specific embodiment
Embodiment 1
The preparation method of denatured conductive mica powder the following steps are included:
1) 40 parts of conductive mica powder, 10 parts of aluminium borate whisker, 20 parts of conductive black, profit according to the number of parts by weight, are weighed
0.4 part and 0.6 part of aminopropyl trimethoxysilane of lubricant base oil is spare；
2) conductive mica powder and aluminium borate whisker are subjected to roasting 6h in 1100 DEG C of vacuum drying ovens after mixing, will roasted
After product is cooled to room temperature, product of roasting is dispersed with chitosan aqueous solution, filters, filtrate is dried；
3) filtrate, conductive black, aminopropyl trimethoxysilane and the lube base oil after step 2) drying are existed
60min is stirred to react under the conditions of 75 DEG C.
Embodiment 2
The preparation method of denatured conductive mica powder the following steps are included:
1) 50 parts of conductive mica powder, 5 parts of aluminium borate whisker, 30 parts of conductive black, lubrication according to the number of parts by weight, are weighed
1.2 parts of oil base oil and 2.4 parts of isopro-pyltriethoxysilane it is spare；
2) conductive mica powder and aluminium borate whisker are subjected to roasting 3h in 1300 DEG C of vacuum drying ovens after mixing, will roasted
After product is cooled to room temperature, product of roasting is dispersed with chitosan aqueous solution, filters, filtrate is dried；
3) filtrate, conductive black, isopro-pyltriethoxysilane and the lube base oil after step 2) drying are existed
30min is stirred to react under the conditions of 85 DEG C.
Embodiment 3
A kind of flame-retardant conductive nylon composite materials, according to the number of parts by weight, including following raw material:
70 parts of nylon 610 resin, 8 parts of nylon 11, embodiment 13 parts of 15 parts of denatured conductive mica powder, aramid fiber, oxygen
Change 2 parts of chromium, 3 parts of zirconium oxide, 3 parts of decabromodiphenylethane, 6 parts of maleic anhydride grafted ethene-octene copolymer, styrene-Malaysia
0.8 part of acid anhydride copolymer and three [2,4 di-tert-butyl-phenyl] phosphite esters.
The preparation method of flame-retardant conductive nylon composite materials, comprising the following steps:
1) first by chromium oxide, zirconium oxide, the denatured conductive mica powder of embodiment 1, nylon 610 resin, nylon 11 and Malaysia
Anhydride grafted ethylene-octene copolymer is uniformly mixed, and prepares master batch with double screw extruder；
2) master batch for obtaining step 1) and aramid fiber, antimony oxide, three [2,4 di-tert-butyl-phenyl] phosphorous acid
Ester, styrene-maleic anhydride copolymer mixing, through melting extrusion in double screw extruder.
Embodiment 4
A kind of flame-retardant conductive nylon composite materials, according to the number of parts by weight, including following raw material:
65 parts of nylon 610 resin, 12 parts of nylon 11, embodiment 22 parts of 10 parts of denatured conductive mica powder, aramid fiber, oxygen
Change 3 parts of chromium, 2 parts of zirconium oxide, 2 parts of triphenyl phosphate, 3 parts of glycidyl methacrylate graft ethylene-octene copolymer, benzene
0.2 part of phosphite ester of 0.4 part of ethylene maleic acid anhydride copolymer and three [2,4 di-tert-butyl-phenyls].
The preparation method of flame-retardant conductive nylon composite materials, comprising the following steps:
1) first by chromium oxide, zirconium oxide, the denatured conductive mica powder of embodiment 2, nylon 610 resin, nylon 11 and methyl
Glycidyl acrylate grafted ethene-octene copolymer is uniformly mixed, and prepares master batch with double screw extruder；
2) master batch for obtaining step 1) and aramid fiber, zinc borate, three [2,4 di-tert-butyl-phenyl] phosphite esters, benzene
Ethylene maleic acid anhydride copolymer mixing, through melting extrusion in double screw extruder.
Embodiment 5
A kind of flame-retardant conductive nylon composite materials, according to the number of parts by weight, including following raw material:
75 parts of nylon 610 resin, 6 parts of nylon 11, embodiment 15 parts of 20 parts of denatured conductive mica powder, aramid fiber, oxygen
1 part of chromium of change, 4 parts of zirconium oxide, 4 parts of triphenyl phosphate, 8 parts of maleic anhydride grafted ethene-octene copolymer, maleic anhydride grafting are poly-
0.8 part of phosphite ester of 1.2 parts of phenylate and three [2,4 di-tert-butyl-phenyls].
The preparation method of flame-retardant conductive nylon composite materials, comprising the following steps:
1) first by chromium oxide, zirconium oxide, the denatured conductive mica powder of embodiment 1, nylon 610 resin, nylon 11 and Malaysia
Anhydride grafted ethylene-octene copolymer is uniformly mixed, and prepares master batch with double screw extruder；
2) master batch for obtaining step 1) and aramid fiber, zinc oxide, three [2,4 di-tert-butyl-phenyl] phosphite esters, horse
Maleic anhydride grafted polyphenylene oxide mixing, through melting extrusion in double screw extruder.
Comparative example 1
A kind of flame-retardant conductive nylon composite materials, according to the number of parts by weight, including following raw material:
65 parts of nylon 610 resin, 6 parts of nylon 11, embodiment 15 parts of 20 parts of denatured conductive mica powder, aramid fiber, phosphorus
4 parts of triphenyl phosphate ester, 8 parts of maleic anhydride grafted ethene-octene copolymer, 1.2 parts of maleic anhydride grafted polyphenylene ether and three [2,4 two
Tert-butyl-phenyl] 0.8 part of phosphite ester.Compared with Example 5, chromium oxide and zirconium oxide are not contained.
Preparation method is substantially the same manner as Example 5, the difference is that not containing chromium oxide and zirconium oxide.
Test example
The flame-retardant conductive nylon of flame-retardant conductive nylon composite materials and comparative example 1 that embodiment 3~5 is prepared is compound
Material carries out performance detection, the results are shown in Table 1:
1 flame-retardant conductive nylon composite materials performance of table
From table 1 it follows that not only flame retardant property is good for the flame-retardant conductive nylon composite materials of embodiment 3-5 preparation, lead
Good electrical property, and mechanical properties strength is high；The nylon of comparative example does not contain chromium oxide and zirconium oxide, in electric conductivity and electrostatic
Aspect is obviously weaker, and illustrating chromium oxide and zirconium oxide, there are coordinative roles with denatured conductive mica powder.
The above is merely preferred embodiments of the present invention, be not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of flame-retardant conductive nylon composite materials, which is characterized in that according to the number of parts by weight, including following raw material:
65~75 parts of nylon 610 resin, 6~12 parts of nylon 11,10~20 parts of denatured conductive mica powder, 2~5 parts of aramid fiber,
1~3 part of chromium oxide, 2~4 parts of zirconium oxide, 2~4 parts of fire retardant, 3~8 parts of toughener, 0.4~1.2 part of compatilizer and anti-oxidant
0.2~0.8 part of agent；The denatured conductive mica powder stone is mainly by conductive mica powder, aluminium borate whisker, conductive black, lubricating oil
Base oil and silane coupling agent are prepared.
2. flame-retardant conductive nylon composite materials according to claim 1, which is characterized in that the denatured conductive mica powder stone
Preparation method the following steps are included:
1) according to the number of parts by weight, weigh 40~50 parts of conductive mica powder, 5~10 parts of aluminium borate whisker, conductive black 20~
30 parts, 0.4~1.2 part of lube base oil and 0.6~2.4 part of silane coupling agent are spare；
2) conductive mica powder and aluminium borate whisker are subjected to 3~6h of roasting in 900~1300 DEG C of vacuum drying ovens after mixing, it will
After product of roasting is cooled to room temperature, product of roasting is dispersed with chitosan aqueous solution, filters, filtrate is dried i.e.
It can；
3) by filtrate, conductive black, silane coupling agent and the lube base oil after step 2) drying in 75~85 DEG C of conditions
Under be stirred to react 30~60min.
3. flame-retardant conductive nylon composite materials according to claim 2, which is characterized in that the silane coupling agent is ammonia third
Base trimethoxy silane or isopro-pyltriethoxysilane.
4. flame-retardant conductive nylon composite materials according to claim 1, which is characterized in that the toughener is selected from maleic acid
At least one of acid anhydride grafted ethene-octene copolymer, glycidyl methacrylate graft ethylene-octene copolymer.
5. flame-retardant conductive nylon composite materials according to claim 1, which is characterized in that the compatilizer, which is selected from, is
At least one of styrene-maleic anhydride copolymer, maleic anhydride grafted polyphenylene ether.
6. flame-retardant conductive nylon composite materials according to claim 1, which is characterized in that the fire retardant is selected from ten bromines two
Vinylbenzene or triphenyl phosphate.
7. flame-retardant conductive nylon composite materials according to claim 1 or 2, which is characterized in that the antioxidant be three [2,
4 di-tert-butyl-phenyls] phosphite ester.
8. the preparation method of flame-retardant conductive nylon composite materials as claimed in any one of claims 1 to 7, which is characterized in that
The following steps are included:
1) first chromium oxide, zirconium oxide, denatured conductive mica powder, nylon 610 resin, nylon 11 are uniformly mixed with toughener, are used
Double screw extruder prepares master batch；
2) master batch that step 1) obtains is mixed with aramid fiber, fire retardant, antioxidant, compatilizer, through double screw extruder
Middle melting extrusion.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811076121.9A CN109265991A (en) | 2018-09-14 | 2018-09-14 | Flame-retardant conductive nylon composite materials and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811076121.9A CN109265991A (en) | 2018-09-14 | 2018-09-14 | Flame-retardant conductive nylon composite materials and preparation method thereof |
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| CN109265991A true CN109265991A (en) | 2019-01-25 |
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