CN109852042A - A kind of nylon composite materials and preparation method thereof of fire-retardant anti-impact high stable - Google Patents
A kind of nylon composite materials and preparation method thereof of fire-retardant anti-impact high stable Download PDFInfo
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- CN109852042A CN109852042A CN201811388683.7A CN201811388683A CN109852042A CN 109852042 A CN109852042 A CN 109852042A CN 201811388683 A CN201811388683 A CN 201811388683A CN 109852042 A CN109852042 A CN 109852042A
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Abstract
The present invention relates to a kind of nylon composite materials and preparation method thereof of fire-retardant anti-impact high stable, nylon composite materials include the component of following parts by weight: 40-60 parts of nylon resins, 40-50 parts of glass fibres, 15-25 parts of DOPO derivative flame retardants, 10-25 parts of polycaprolactones, 2-10 parts of toughener, 0.05-0.1 parts of crystallization nucleating agents, 0.01-0.05 parts of crystallization promoters, 1-5 parts of lubricants, 0.3-1 parts of antioxidant.The nylon composite materials flame retardant properties, mechanical properties of fire-retardant anti-impact high stable of the invention, thermo-oxidative stability are good, and processing performance is good.
Description
Technical field
The present invention relates to a kind of nylon composite materials and preparation method thereof of fire-retardant anti-impact high stable, belong to high molecular material
Technical field.
Background technique
Nylon (PA) is the thermoplastic resin general name containing recurring amide radical group on molecular backbone, with excellent wear-resisting
Property, corrosion resistance and preferable molding processibility, but fire retardancy is poor, and the more PA fire retardant of dosage mainly has halogen system at present
With inorganic metal compound etc., but there are the problems such as expensive, processing difficulties, pollution be big for these fire retardants, have
Resin material poor fluidity, color can be also set to be deteriorated, wherein the bromine system small molecule fire retardant that industrial dosage is most, due to its combustion
After burning product it is larger to environmental hazard and have dispute.In addition, the impact resistance under the thermo-oxidative stability of nylon material, cryogenic conditions
Intensity and dimensional stability Shortcomings, make its popularization and use by certain limitation.
In recent years, the application with nylon in the fields such as automobile, electronics, electrical, communication is more and more wider, as electric appliance member portion
New material in part proprietary material, to the fire retardancy of nylon material, thermo-oxidative stability, impact resistant strength and dimensional stability etc.
Performance requirement is also higher and higher.
Summary of the invention
The technical problem to be solved by the present invention is to solve existing nylon resin fire retardancy, thermo-oxidative stability, low temperature item
The poor technical problem of impact resistant strength and dimensional stability under part, provides a kind of nylon composite wood of fire-retardant anti-impact high stable
Material and preparation method thereof.
The technical solution adopted by the present invention to solve the technical problems is:
A kind of nylon composite materials of fire-retardant anti-impact high stable, the component including following parts by weight: 40-60 parts of nylon trees
Rouge, 40-50 parts of glass fibres, 15-25 parts of DOPO derivative flame retardants, 10-25 parts of polycaprolactones, 2-10 parts of toughener, 0.05-
0.1 part of crystallization nucleating agent, 0.01-0.05 parts of crystallization promoters, 1-5 parts of lubricants, 0.3-1 parts of antioxidant；The DOPO is derivative
The structural formula of object fire retardant is as follows:R is
Preferably, the nylon resin is 20-30 parts of PA66,20-30 parts of PA6.
Preferably, the toughener is the soft core-shell copolymerized object of core hard-shell type, and the soft core-shell copolymerized object of core hard-shell type is first
The core-shell copolymerized object of base methyl acrylate-acrylic acid butyl ester, organic-silicon-modified methyl methacrylate-butyl acrylate are core-shell copolymerized
At least one of object, methylacrylate- butadiene-styrene core-shell copolymer.
Preferably, the crystallization nucleating agent is 4,6- di-tert-butyl based phosphates and/or 1,3,5- n-butylbenzene front threes
Amide.
Preferably, the crystallization promoter is 1,3:2,4- bis- (3,4- dimethyl) benzylidene sorbitol acetal, tri- Benzyl base fork
One of propyl ether dibasic acid esters hexanol, neopentyl ethylene glycol Biphenyl Ester are a variety of.
Preferably, the antioxidant is the composition of Hinered phenols antioxidant and phosphite ester antioxidant.
Preferably, the Hinered phenols antioxidant be β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid octadecanol ester,
Four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters or 4, (3, the 5- di-t-butyl -4- hydroxyl benzyls of 6- tri-
Base) benzene.
Preferably, the phosphite ester antioxidant is three [2,4- di-tert-butyl-phenyl] phosphite esters or bis- (2,4- bis-
Tert-butyl phenol) pentaerythritol diphosphites.
Preferably, the nylon composite materials of the fire-retardant anti-impact high stable further include the black masterbatch of 1-5 parts by weight, described black
Master batch is preferably Cabot black masterbatch.
Preferably, the lubricant is the mixture of TAF and calcium stearate, and the mass ratio of the TAF and calcium stearate is 2
∶3-3∶2。
Preferably, the single fiber diameter of the glass fibre be 9.9~12.1 μm, water content≤0.10%, be chopped rate >=
98.00%, 3.5~5.5mm of chopped length.
The present invention also provides a kind of preparation method of the nylon composite materials of fire-retardant anti-impact high stable, preparation step is as follows:
By nylon resin, glass fibre, DOPO derivative flame retardant, polycaprolactone, toughener, crystallization nucleating agent, crystallization
Promotor, lubricant and antioxidant are blended uniformly, obtain premix raw material, then add twin-screw extrude premix raw material mixed
Refining is squeezed out, is granulated, and obtains the nylon composite materials of fire-retardant anti-impact high stable；The extrusion temperature of the double screw extruder is preferably
220-255℃。
The beneficial effects of the present invention are:
(1) nylon composite materials of fire-retardant anti-impact high stable of the invention are using DOPO derivative as fire retardant, the resistance
Fire agent Halogen, smokeless, nontoxic, flame retardant property is more preferable, more longlasting, the polycaprolactone of addition can reduce nylon composite materials plus
Work temperature, ensure that the thermal stability of fire retardant, and the melt flow rate (MFR) of nylon composite materials can be improved, and it is multiple to improve nylon
The processing performance of condensation material.
(2) nylon composite materials of fire-retardant anti-impact high stable of the invention use the soft core using methyl methacrylate as shell
The core-shell copolymerized object of hard-shell type improves the mechanical property of nylon composite materials, ensure that nylon composite materials as toughener
Dimensional stability.
(3) nylon composite materials of fire-retardant anti-impact high stable of the invention use crystallization nucleating agent and crystallization promoter, two
Person synergistic effect can significant increase nylon crystallization rate, the crystal being formed simultaneously is small and more, improve nylon crystallinity and
Thermo-oxidative stability.
(4) nylon composite materials of fire-retardant anti-impact high stable of the invention select the mixture of TAF and calcium stearate as
Lubricant, TAF form similar anchoring node between glass fibre and matrix resin, and TAF and calcium stearate synergistic effect can
It is effectively improved the caking property and dispersibility of glass fibre and matrix resin, glass fibre exposing phenomenon is effectively prevent, can also improve
Fire retardant is evenly dispersed in matrix resin.
(5) present invention selection Hinered phenols antioxidant and phosphite ester antioxidant are used cooperatively, and the antioxidant of compounding exists
Anti-oxidant aspect is complementary to one another, and can cooperate with the thermo-oxidative stability for improving nylon composite materials each component.
Specific embodiment
The present invention is described in further detail now.
Embodiment 1
The present embodiment provides a kind of nylon composite materials of fire-retardant anti-impact high stable, the components including following parts by weight: 20
Part PA66,30 parts of PA6,40 parts of glass fibres, 15 parts of DOPO derivative flame retardants, 10 parts of polycaprolactones, 2 parts of toughener (methyl
The core-shell copolymerized object of methyl acrylate-acrylic acid butyl ester), 0.05 part of crystallization nucleating agent (4,6- di-tert-butyl-phenyl ammonium phosphate),
0.01 part of crystallization promoter (1,3:2,4- bis- (3,4- dimethyl) benzylidene sorbitol acetal), 1 part of lubricant (mass ratio 2: 3
TAF and calcium stearate), 0.3 part of antioxidant (0.1 part of β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid octadecanol ester,
0.2 part of three [2,4- di-tert-butyl-phenyl] phosphite ester)；The structural formula of the DOPO derivative flame retardant is as follows:The R isThe single fiber diameter of the glass fibre be 9.9~12.1 μm, it is aqueous
Amount≤0.10%, be chopped rate >=98.00%, 3.5~5.5mm of chopped length.
The nylon composite materials of the fire-retardant anti-impact high stable the preparation method is as follows:
By nylon resin, glass fibre, DOPO derivative flame retardant, polycaprolactone, toughener, crystallization nucleating agent, crystallization
Promotor, lubricant and antioxidant are stirred 10 minutes with the speed of 500r/min, obtain premix raw material；
Premix raw material is added twin-screw extrude into mixing, extrusion, granulation, the nylon for obtaining fire-retardant anti-impact high stable is compound
Material, double screw extruder temperature of each section setting are as follows: 220 DEG C of an area, 235 DEG C of 2nd area, 240 DEG C of 3rd area, 250 DEG C of 4th area, 5th area
255 DEG C, 250 DEG C of 6th area, 245 DEG C of 7th area, 240 DEG C of 8th area, 235 DEG C of 9th area, 230 DEG C of tenth area, 225 DEG C of 11st area, head 250
DEG C, engine speed 400r/min, feeding frequency 10r/min.
Embodiment 2
The present embodiment provides a kind of nylon composite materials of fire-retardant anti-impact high stable, the components including following parts by weight: 30
Part PA66,20 parts of PA6,50 parts of glass fibres, 25 parts of DOPO derivative flame retardants, 25 parts of polycaprolactones, 10 parts of toughener are (organic
The core-shell copolymerized object of Si modification methyl methacrylate-butyl acrylate), 0.1 part of crystallization nucleating agent (1,3,5- n-butylbenzene front three
Amide), 0.05 part of crystallization promoter (tri- Benzyl base pitches propyl ether dibasic acid esters hexanol), 5 parts of lubricant (TAF and tristearin of mass ratio 3: 2
Sour calcium), 1 part of antioxidant (0.5 part of four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, 0.5 part it is bis- (2,
4- DI-tert-butylphenol compounds) pentaerythritol diphosphites), 1 part of Cabot black masterbatch；The structure of the DOPO derivative flame retardant
Formula is as follows:The R isThe single fiber diameter of the glass fibre is 9.9
~12.1 μm, water content≤0.10%, chopped rate >=98.00%, 3.5~5.5mm of chopped length.
The preparation method is the same as that of Example 1 for the nylon composite materials of the fire-retardant anti-impact high stable.
Embodiment 3
The present embodiment provides a kind of nylon composite materials of fire-retardant anti-impact high stable, the components including following parts by weight: 25
Part PA66,25 parts of PA6,45 parts of glass fibres, 20 parts of DOPO derivative flame retardants, 20 parts of polycaprolactones, 5 parts of toughener (methyl
Methylacrylate-butadiene-styrene nucleocapsid copolymer), 0.08 part of crystallization nucleating agent (0.04 part of 4,6- di-tert-butyl-phenyl phosphorus
Hydrochlorate and 0.04 part 1,3,5- n-butylbenzene trimethamides), 0.03 part of crystallization promoter (neopentyl ethylene glycol Biphenyl Ester), 1 part
Lubricant (TAF and calcium stearate of mass ratio 1: 1), 0.6 part of antioxidant (0.3 part of (3,5- di-t-butyl -4- hydroxyl of 4,6- tri-
Base benzyl) benzene, 0.3 part of three [2,4- di-tert-butyl-phenyl] phosphite ester), 5 parts of Cabot black masterbatch；The DOPO derivative resistance
The structural formula for firing agent is as follows:The R isThe single fiber of the glass fibre
Diameter is 9.9~12.1 μm, water content≤0.10%, be chopped rate >=98.00%, 3.5~5.5mm of chopped length.
The preparation method is the same as that of Example 1 for the nylon composite materials of the fire-retardant anti-impact high stable.
Embodiment 4
The present embodiment provides a kind of nylon composite materials of fire-retardant anti-impact high stable, the components including following parts by weight: 20
Part PA66,30 parts of PA6,40 parts of glass fibres, 20 parts of DOPO derivative flame retardants, 10 parts of polycaprolactones, 8 parts of toughener (methyl
The core-shell copolymerized object of methyl acrylate-acrylic acid butyl ester), 0.06 part of crystallization nucleating agent (4,6- di-tert-butyl-phenyl ammonium phosphate),
0.02 part of crystallization promoter (1,3:2,4- bis- (3,4- dimethyl) benzylidene sorbitol acetal), 2 parts of lubricant (mass ratioes 1: 1
TAF and calcium stearate), 0.7 part of antioxidant (0.5 part of β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid octadecanol ester,
0.2 part of three [2,4- di-tert-butyl-phenyl] phosphite ester), 4 parts of Cabot black masterbatch；The structure of the DOPO derivative flame retardant
Formula is as follows:The R isThe single fiber diameter of the glass fibre be 9.9~
12.1 μm, water content≤0.10%, chopped rate >=98.00%, 3.5~5.5mm of chopped length.
The preparation method is the same as that of Example 1 for the nylon composite materials of the fire-retardant anti-impact high stable.
Embodiment 5
The present embodiment provides a kind of nylon composite materials of fire-retardant anti-impact high stable, the components including following parts by weight: 23
Part PA66,28 parts of PA6,42 parts of glass fibres, 18 parts of DOPO derivative flame retardants, 12 parts of polycaprolactones, 5 parts of toughener (methyl
The core-shell copolymerized object of methyl acrylate-acrylic acid butyl ester), 0.07 part of crystallization nucleating agent (4,6- di-tert-butyl-phenyl ammonium phosphate),
0.02 part of crystallization promoter (1,3:2,4- bis- (3,4- dimethyl) benzylidene sorbitol acetal), 2 parts of lubricant (mass ratioes 2: 3
TAF and calcium stearate), 0.5 part of antioxidant (0.1 part of β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid octadecanol ester,
0.4 part of three [2,4- di-tert-butyl-phenyl] phosphite ester), 2 parts of Cabot black masterbatch；The structure of the DOPO derivative flame retardant
Formula is as follows:The R isThe single fiber diameter of the glass fibre is 9.9~12.1
μm, water content≤0.10%, be chopped rate >=98.00%, 3.5~5.5mm of chopped length.
The preparation method is the same as that of Example 1 for the nylon composite materials of the fire-retardant anti-impact high stable.
Embodiment 6
The present embodiment provides a kind of nylon composite materials of fire-retardant anti-impact high stable, the components including following parts by weight: 28
Part PA66,23 parts of PA6,48 parts of glass fibres, 22 parts of DOPO derivative flame retardants, 20 parts of polycaprolactones, 8 parts of toughener (methyl
Methylacrylate-butadiene-styrene nucleocapsid copolymer), 0.08 part of crystallization nucleating agent (1,3,5- n-butylbenzene trimethamide),
0.03 part of crystallization promoter (tri- Benzyl base pitches propyl ether dibasic acid esters hexanol), 4 parts of lubricants (TAF and calcium stearate of mass ratio 3: 2),
0.8 part of antioxidant (0.4 part of β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid octadecanol ester, 0.4 part of three [tertiary fourth of 2,4- bis-
Base phenyl] phosphite ester), 3 parts of Cabot black masterbatch；The structural formula of the DOPO derivative flame retardant is as follows:The R isThe single fiber diameter of the glass fibre is 9.9~12.1 μ
M, water content≤0.10%, chopped rate >=98.00%, 3.5~5.5mm of chopped length.
The preparation method is the same as that of Example 1 for the nylon composite materials of the fire-retardant anti-impact high stable.
The properties of product of embodiment 1-6 are tested, with the tensile strength of 527 test product of standard ISO, with standard
The bending strength of 178 test product of ISO, with the notch impact strength of standard ISO 179~1eA test product, with standard ISO
The heat distortion temperature of 75 test products, with the hardness of 2039 test product of standard ISO, with the fire-retardant of standard UL94 test product
Grade.The properties of product test result of embodiment 1-6 is as shown in table 1.
The properties of product test result of 1 embodiment 1-6 of table
Taking the above-mentioned ideal embodiment according to the present invention as inspiration, through the above description, relevant staff is complete
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention
Property range is not limited to the contents of the specification, it is necessary to which the technical scope thereof is determined according to the scope of the claim.
Claims (10)
1. a kind of nylon composite materials of fire-retardant anti-impact high stable, which is characterized in that the component including following parts by weight: 40-60
Part nylon resin, 40-50 parts of glass fibres, 15-25 parts of DOPO derivative flame retardants, 10-25 parts of polycaprolactones, 2-10 parts of toughenings
Agent, 0.05-0.1 parts of crystallization nucleating agents, 0.01-0.05 parts of crystallization promoters, 1-5 parts of lubricants, 0.3-1 parts of antioxidant；It is described
The structural formula of DOPO derivative flame retardant is as follows:R is
2. the nylon composite materials of fire-retardant anti-impact high stable according to claim 1, which is characterized in that the nylon resin
For 20-30 parts of PA66,20-30 parts of PA6.
3. the nylon composite materials of fire-retardant anti-impact high stable according to claim 1 or 2, which is characterized in that the toughening
Agent is the soft core-shell copolymerized object of core hard-shell type, and the soft core-shell copolymerized object of core hard-shell type is methyl methacrylate-butyl acrylate
Core-shell copolymerized object, the core-shell copolymerized object of organic-silicon-modified methyl methacrylate-butyl acrylate, methyl methacrylate-fourth two
At least one of alkene-styrene nucleocapsid copolymer.
4. the nylon composite materials of fire-retardant anti-impact high stable according to claim 1-3, which is characterized in that described
Crystallization nucleating agent is 4,6- di-tert-butyl based phosphates and/or 1,3,5- n-butylbenzene trimethamides.
5. the nylon composite materials of fire-retardant anti-impact high stable according to claim 1-4, which is characterized in that described
Crystallization promoter is that 1,3:2,4- bis- (3,4- dimethyl) benzylidene sorbitol acetal, tri- Benzyl base pitches propyl ether dibasic acid esters hexanol, neopentyl
One of ethylene glycol Biphenyl Ester is a variety of.
6. the nylon composite materials of fire-retardant anti-impact high stable according to claim 1-5, which is characterized in that described
Antioxidant is the composition of Hinered phenols antioxidant and phosphite ester antioxidant, and the Hinered phenols antioxidant is β-(3,5-
Di-tert-butyl-hydroxy phenyl) propionic acid octadecanol ester, four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] Ji Wusi
Alcohol ester or 4,6- tri- (3,5- di-tert-butyl-4-hydroxyl benzyl) benzene, the phosphite ester antioxidant are three [2,4- di-t-butyls
Phenyl] phosphite ester or bis- (2,4- DI-tert-butylphenol compounds) pentaerythritol diphosphites.
7. the nylon composite materials of fire-retardant anti-impact high stable according to claim 1-6, which is characterized in that described
The nylon composite materials of fire-retardant anti-impact high stable further include the black masterbatch of 1-5 parts by weight, and the black masterbatch is preferably that Cabot is black
Master batch.
8. the nylon composite materials of fire-retardant anti-impact high stable according to claim 1-7, which is characterized in that described
Lubricant is the mixture of TAF and calcium stearate, and the mass ratio of the TAF and calcium stearate is 2: 3-3: 2.
9. the nylon composite materials of fire-retardant anti-impact high stable according to claim 1-8, which is characterized in that described
The single fiber diameter of glass fibre is 9.9~12.1 μm, water content≤0.10%, be chopped rate >=98.00%, chopped length 3.5
~5.5mm.
10. a kind of preparation method of the nylon composite materials of the described in any item fire-retardant anti-impact high stables of claim 1-9, special
Sign is that preparation step is as follows:
Nylon resin, glass fibre, DOPO derivative flame retardant, polycaprolactone, toughener, crystallization nucleating agent, crystallization are promoted
Agent, lubricant and antioxidant are blended uniformly, obtain premix raw material, and premix raw material is then added twin-screw extrude mixing, is squeezed
Out, it is granulated, obtains the nylon composite materials of fire-retardant anti-impact high stable；The extrusion temperature of the double screw extruder is preferably 220-
255℃。
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| CN201811388683.7A CN109852042A (en) | 2018-11-21 | 2018-11-21 | A kind of nylon composite materials and preparation method thereof of fire-retardant anti-impact high stable |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111041569A (en) * | 2019-12-16 | 2020-04-21 | 中山市冠一织带有限公司 | Flame-retardant reinforced polyester yarn, woven tape and preparation method |
| CN112457663A (en) * | 2020-10-31 | 2021-03-09 | 山东广垠新材料有限公司 | Flame-retardant nylon corrugated pipe modified material and preparation method thereof |
| CN117363003A (en) * | 2023-11-14 | 2024-01-09 | 金发科技股份有限公司 | Halogen-free flame-retardant polyamide composite material and preparation method and application thereof |
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| CN102134378A (en) * | 2010-01-21 | 2011-07-27 | 顾红军 | Polyester composite material with controllable crystallinity for sheet material |
| CN102875982A (en) * | 2012-10-15 | 2013-01-16 | 宁波优科泰科技发展有限公司 | In-situ modified halogen-free flame retardant thermoplastic resin composition and preparation method thereof |
| CN108456419A (en) * | 2018-05-10 | 2018-08-28 | 南京跃贝新材料科技有限公司 | A kind of low viscosity exempts from spray metal silver color daiamid composition and preparation method thereof |
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| CN102134378A (en) * | 2010-01-21 | 2011-07-27 | 顾红军 | Polyester composite material with controllable crystallinity for sheet material |
| CN102875982A (en) * | 2012-10-15 | 2013-01-16 | 宁波优科泰科技发展有限公司 | In-situ modified halogen-free flame retardant thermoplastic resin composition and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111041569A (en) * | 2019-12-16 | 2020-04-21 | 中山市冠一织带有限公司 | Flame-retardant reinforced polyester yarn, woven tape and preparation method |
| CN112457663A (en) * | 2020-10-31 | 2021-03-09 | 山东广垠新材料有限公司 | Flame-retardant nylon corrugated pipe modified material and preparation method thereof |
| CN117363003A (en) * | 2023-11-14 | 2024-01-09 | 金发科技股份有限公司 | Halogen-free flame-retardant polyamide composite material and preparation method and application thereof |
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Application publication date: 20190607 |