CN106543630A - A kind of flame-proof heat-resistant type automobile plastic uptake material of containing mesopore molecular sieve Graphene and preparation method thereof - Google Patents
A kind of flame-proof heat-resistant type automobile plastic uptake material of containing mesopore molecular sieve Graphene and preparation method thereof Download PDFInfo
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- CN106543630A CN106543630A CN201610934214.5A CN201610934214A CN106543630A CN 106543630 A CN106543630 A CN 106543630A CN 201610934214 A CN201610934214 A CN 201610934214A CN 106543630 A CN106543630 A CN 106543630A
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- molecular sieve
- graphene
- resin
- flame
- mesopore molecular
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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
- C08L55/00—Compositions of homopolymers or copolymers, obtained by polymerisation reactions only involving carbon-to-carbon unsaturated bonds, not provided for in groups C08L23/00 - C08L53/00
- C08L55/02—ABS [Acrylonitrile-Butadiene-Styrene] polymers
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- 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
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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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
- 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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
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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
- C08L2205/04—Polymer mixtures characterised by other features containing interpenetrating networks
Abstract
The invention discloses a kind of flame retardant automotive plastic uptake material of containing mesopore molecular sieve Graphene, and its preparation technology, characterized in that, with acrylonitrile butadient styrene (ABS), linear phenol-aldehyde resin, microcapsule red phosphorus, alkali magnesium sulfate crystal whisker, nitrile rubber, mesopore molecular sieve SBA 15, APP, melamine resin, Kaolin, Sb2O3, dimethicone, Graphene etc. be raw material.Intermediary's porous molecular sieve of the present invention produces bonded effect with linear phenolic resin, improves matrix resin heat stability；Micro encapsulation APP and Ultrafine Antimony-Oxide/Kaolin Composite Powder produce cooperative effect, and flame retardant effect is more preferably；Graphene is added in ABS resin matrix, hence it is evident that improve the anti-flammability and heat stability of resin, and mechanical property is also higher；Obtain a kind of flame retardant automotive plastic uptake material of containing mesopore molecular sieve Graphene.
Description
Technical field
The present invention relates to the field of fire-proof technology of composite, and in particular to a kind of resistance of containing mesopore molecular sieve-Graphene
Combustion heat resistant type automobile plastic uptake material, and its preparation technology.
Background technology
The terpolymer that ABS is made up of acrylonitrile, butadiene and styrene, as a kind of thermoplastic engineering plastic,
With its excellent mechanical property, chemical inertness and workability, auto industry, electronics, electrical equipment, weaving, device are widely used in
The field such as tool and building materials.But the fire resistance of ABS resins is poor, a kind of additive how is found, ABS resin can be made
While fire resistance is improved, and reduce the premium properties of itself, become the focus of research.
Yang Bing is in Master's thesis《Research based on linear phenol-aldehyde resin and microcapsule red phosphorus halogen-free flame retardant ABS》Profit in one text
With the low cigarette of low toxicity, high temperature resistant, high fixing carbon, economical and efficient linear phenol-aldehyde resin as carbon forming agent, assisted with microencapsulated powder oil
With fire-retardant, with alkali magnesium sulfate crystal whisker as inorganic combustion inhibitor, select and increased with the preferable nitrile rubber of the ABS matrix compatibilitys
It is tough modified, antioxidant and mixed uniformly line style are sequentially added after when experiment plastify ABS in 180 DEG C of two-roll mill
Phenolic resin, microcapsule red phosphorus, inorganic combustion inhibitor alkali magnesium sulfate crystal whisker, nitrile rubber blends, discharge simultaneously after mixing is uniform
It is positioned in mould, hot pressing 10 minutes, then colds pressing 10 minutes at room temperature on 180 DEG C of the vulcanizing press, depanning is obtained
Modified ABS plastic sheet material, but it is not enough to there is flame retardant effect.
The present invention on this basis, produces bonded effect with linear phenolic resin by mesopore molecular sieve, and strand runs through
Inside and outside the duct of mesopore molecular sieve, organic-inorganic hybrid material is formed, matrix resin heat stability is improve；With in-situ polymerization
Method is prepared for micro encapsulation APP；Ultrafine Antimony-Oxide/Kaolin Composite Powder is prepared for ball-milling method；Graphene is added to
In ABS resin matrix, hence it is evident that improve the anti-flammability and heat stability of resin, mechanical property is also higher；Using filling-modified method
Filler Pulvis Talci is added in ABS, improves the thermostability of ABS；Obtain a kind of flame-proof heat-resistant of containing mesopore molecular sieve-Graphene
Type automobile plastic uptake material.
The content of the invention
The invention mainly solves the technical problem of providing a kind of flame-proof heat-resistant type automobile of containing mesopore molecular sieve-Graphene
Plastic uptake material and its preparation technology, the automobile plastic uptake material made according to the technique have light weight, heat-resisting, fire protection flame retarding it is excellent
Performance.
The technical problem to be solved is realized using following technical scheme：
Acrylonitrile-butadiene-styrene copolymer (ABS) 42-50, linear phenol-aldehyde resin 4-9, microcapsule red phosphorus 5-9, alkali formula
Magnesium sulfate crystal whisker 2-5, nitrile rubber 3-5, mesoporous molecular sieve SBA-15 6-10, APP 5-8, melamine resin
2-4, Kaolin 1-3, Sb2O33-8, dimethicone 1-3, Graphene 5-8, precipitated calcium carbonate 5-10, potassium titanate crystal whisker 2-5, liquid
Body paraffin 1-2, superfine talcum powder 3-5, ethanol, distilled water, appropriate acetic acid.
A kind of preparation method of the flame-proof heat-resistant type automobile plastic uptake material of containing mesopore molecular sieve-Graphene, it is characterised in that
Carry out according to the following steps：
A. mesoporous molecular sieve SBA-15 is mixed with linear phenol-aldehyde resin, after reacting 1-3h at 180-190 DEG C,
Microcapsule red phosphorus are added, is continued reaction 1-2h, product is placed in dehydrated alcohol, 25-40 DEG C of stirring 10-12h, second
Alcohol dissolves unreacted resin, filters, alcohol is washed, dry hybrid material；
B. in APP 1:2-3 adds ethanol and distilled water, after dispersed with stirring 10-30min, adds melamino-formaldehyde
Resin, it is 4-5 to adjust pH with acetic acid, is warming up to 80-90 DEG C of stirring reaction 2-3h, sucking filtration, washing, it is dry not exclusively coat it is micro-
Encapsulated APP；
C. 1-2h, and Sb are calcined in Kaolin grinding washing after 600-900 DEG C2O3Mixing, is placed in water ultrasonic disperse and makes
Serosity, is put into baking oven after ball milling 4-6h, in 110-130 DEG C of drying 5-8h, obtains composite micro-powder, and which is mixed with resulting material in b
Uniformly, add dimethicone at 60-120 DEG C, whip modified 15-60min, sucking filtration, washing, dry composite flame-retardant agent；
D. ABS resin is added in 180-190 DEG C of two-roll mill and is plastified, after ABS resin into after molten condition, then plus
The hybrid material obtained in entering Graphene and a, must knead material after mixing 10-40min；
E. precipitated calcium carbonate is dried into 1-2h at 80-100 DEG C, then by itself and potassium titanate crystal whisker, liquid paraffin, ultra-fine cunning
Stone powder mixes 20-50min, then resulting material in d is added thereto, and mixes 1-2h；
F. the composite flame-retardant agent in c, the mixing material in e and other residual componentss are blended at 185-195 DEG C, mixing is equal
Discharge after even and be positioned in mould, the hot pressing 10-30min on 180-190 DEG C of the vulcanizing press, then cold pressing at room temperature
10-30min, depanning are obtained modified ABS plastic sheet material, that is, obtain a kind of flame-proof heat-resistant type of containing mesopore molecular sieve-Graphene
Automobile plastic uptake material.
The present invention reaction mechanism and have the beneficial effect that：
（1）Mesopore molecular sieve/linear phenol-aldehyde resin organic-inorganic hybrid material, linear phenol are prepared for by the method for in-situ polymerization
Urea formaldehyde is distributed in inside and outside mesopore molecular sieve duct, and there is bonded effect with SBA-15, forms organic-inorganic interpenetrating networks knot
Structure, improves matrix resin heat stability.
（2）Micro encapsulation APP is prepared with situ aggregation method（MCAPP）, APP after cladding, can be significantly reduced
（APP）Water solubility and hygroscopicity, improve the resistance to leaching and limited oxygen index of material, melamine resin（MF）
There is good synergism with APP, in the case of APP claddings are incomplete, can more effectively play both interactions,
Improve the anti-flammability of composite.
（3）Sb is prepared for ball-milling method2O3/ Kaolin composite flame-proof micropowder, Sb2O3Belong to additive flame retardant, with stibium trioxide
Based on powder, Kaolin is attached to stibium trioxide powder surface, and physics, chemical action occur with stibium trioxide powder fully；
It is used in combination with APP, produces cooperative effect, flame retardant effect is more preferably.
（4）Graphene as the new lover in material with carbon element family, with incomparable excellent performance, can as the additive of ABS,
Graphene is added in ABS resin matrix, hence it is evident that improve the anti-flammability and heat stability of resin, mechanical property is also higher.
（5）Filler Pulvis Talci is added in ABS using filling-modified method, improves the thermostability of ABS.
Specific embodiment
In order that technological means, creation characteristic, reached purpose and effect that the present invention is realized are easy to understand, tie below
Specific embodiment is closed, the present invention is expanded on further.
Embodiment
The flame-proof heat-resistant type automobile plastic uptake material of a kind of containing mesopore molecular sieve-Graphene, by the raw material of following weight parts (g)
It is obtained：
Acrylonitrile-butadiene-styrene copolymer (ABS) 48, linear phenol-aldehyde resin 6, microcapsule red phosphorus 5, alkali magnesium sulfate are brilliant
Palpus 2, nitrile rubber 3, mesoporous molecular sieve SBA-15 6, APP 5, melamine resin 2, Kaolin 1, Sb2O33, two
Methyl-silicone oil 1, Graphene 5, precipitated calcium carbonate 6, potassium titanate crystal whisker 2, liquid paraffin 1, superfine talcum powder 3, ethanol, distilled water,
Appropriate acetic acid.
A kind of preparation method of the flame-proof heat-resistant type automobile plastic uptake material of containing mesopore molecular sieve-Graphene, it is characterised in that
Carry out according to the following steps：
A. mesoporous molecular sieve SBA-15 is mixed with linear phenol-aldehyde resin, after 1h being reacted at 180 DEG C, add microcapsule red phosphorus,
Continue reaction 2h, product is placed in dehydrated alcohol, 40 DEG C of stirring 10h, ethanol dissolve unreacted resin, filtration, alcohol
Wash three times, dry hybrid material；
B. in APP 1:2 add ethanol and distilled water, after dispersed with stirring 10min, add melamine resin,
Adjust pH to 5 with acetic acid, be warming up to 80 DEG C of stirring reactions 3h, sucking filtration, washing, dry the micro encapsulation polyphosphoric acid for not exclusively coating
Ammonium；
C. 1h, and Sb are calcined in Kaolin grinding washing after 750 DEG C2O3Mixing, is placed in water ultrasonic disperse and makes serosity,
Baking oven is put into after ball milling 4h, in 130 DEG C of dryings 5h, composite micro-powder is obtained, which is mixed homogeneously with resulting material in b, at 80 DEG C
Add dimethicone, whip modified 30min, sucking filtration, washing, dry composite flame-retardant agent；
D. ABS resin is added in 185 DEG C of two-roll mill and is plastified, after ABS resin into after molten condition, add stone
The hybrid material obtained in black alkene and a, must knead material after mixing 20min；
E. precipitated calcium carbonate is dried into 1h at 90-100 DEG C, then by itself and potassium titanate crystal whisker, liquid paraffin, extra fine talc
Powder mixes 40-50min, then resulting material in d is added thereto, and mixes 2h；
F. the composite flame-retardant agent in c, the mixing material in e and other residual componentss are blended at 185 DEG C, after mixing is uniform
Discharge and be positioned in mould, the hot pressing 20min on 180 DEG C of the vulcanizing press, then the 30min that colds pressing at room temperature, go out molding
The ABS plastic sheet material that must be modified, that is, obtain a kind of flame-proof heat-resistant automobile plastic uptake material of containing mesopore molecular sieve-Graphene.
A kind of performance of the flame-proof heat-resistant type automobile plastic uptake material of containing mesopore molecular sieve-Graphene prepared by above-described embodiment
Testing result is as follows：
Up to UL-94 V-0 levels, LOI values 33%, carbon yield (600 DEG C) 20%, tensile strength reaches the vertical combustion performance of flame-proof ABS
45MPa, notch impact strength are 27 KJ/m2, elongation at break 44%.
Claims (2)
1. the flame-proof heat-resistant type automobile plastic uptake material of a kind of containing mesopore molecular sieve-Graphene, it is characterised in that by following weight parts
Raw material be obtained：
Acrylonitrile-butadiene-styrene copolymer (ABS) 42-50, linear phenol-aldehyde resin 4-9, microcapsule red phosphorus 5-9, alkali formula
Magnesium sulfate crystal whisker 2-5, nitrile rubber 3-5, mesoporous molecular sieve SBA-15 6-10, APP 5-8, melamine resin
2-4, Kaolin 1-3, Sb2O33-8, dimethicone 1-3, Graphene 5-8, precipitated calcium carbonate 5-10, potassium titanate crystal whisker 2-5, liquid
Body paraffin 1-2, superfine talcum powder 3-5, ethanol, distilled water, appropriate acetic acid.
2. the system of the flame-proof heat-resistant type automobile plastic uptake material of a kind of containing mesopore molecular sieve-Graphene according to claim 1
Preparation Method, it is characterised in that carry out according to the following steps：
Mesoporous molecular sieve SBA-15 is mixed with linear phenol-aldehyde resin, after 1-3h being reacted at 180-190 DEG C, adds microcapsule red
Phosphorus, continues reaction 1-2h, product is placed in dehydrated alcohol, and 25-40 DEG C of stirring 10-12h, ethanol dissolve unreacted tree
Fat, filters, alcohol is washed, dry hybrid material；
B. in APP 1:2-3 adds ethanol and distilled water, after dispersed with stirring 10-30min, adds melamino-formaldehyde
Resin, it is 4-5 to adjust pH with acetic acid, is warming up to 80-90 DEG C of stirring reaction 2-3h, sucking filtration, washing, it is dry not exclusively coat it is micro-
Encapsulated APP；
C. 1-2h, and Sb are calcined in Kaolin grinding washing after 600-900 DEG C2O3Mixing, is placed in water ultrasonic disperse and makes
Serosity, is put into baking oven after ball milling 4-6h, in 110-130 DEG C of drying 5-8h, obtains composite micro-powder, and which is mixed with resulting material in b
Uniformly, add dimethicone at 60-120 DEG C, whip modified 15-60min, sucking filtration, washing, dry composite flame-retardant agent；
D. ABS resin is added in 180-190 DEG C of two-roll mill and is plastified, after ABS resin into after molten condition, then plus
The hybrid material obtained in entering Graphene and a, must knead material after mixing 10-40min；
E. precipitated calcium carbonate is dried into 1-2h at 80-100 DEG C, then by itself and potassium titanate crystal whisker, liquid paraffin, ultra-fine cunning
Stone powder mixes 20-50min, then resulting material in d is added thereto, and mixes 1-2h；
F. the composite flame-retardant agent in c, the mixing material in e and other residual componentss are blended at 185-195 DEG C, mixing is equal
Discharge after even and be positioned in mould, the hot pressing 10-30min on 180-190 DEG C of the vulcanizing press, then cold pressing at room temperature
10-30min, depanning are obtained modified ABS plastic sheet material, that is, obtain a kind of flame-proof heat-resistant type of containing mesopore molecular sieve-Graphene
Automobile plastic uptake material.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107146922A (en) * | 2017-04-11 | 2017-09-08 | 航美（深圳）新能源科技有限公司 | A kind of fire-retardant cellular adaptive temperature control module and preparation method thereof, application |
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| CN105482349A (en) * | 2014-10-10 | 2016-04-13 | 西安艾菲尔德复合材料科技有限公司 | High temperature resistant halogen-free flame retardant ABS composition |
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2016
- 2016-10-25 CN CN201610934214.5A patent/CN106543630A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107146922A (en) * | 2017-04-11 | 2017-09-08 | 航美（深圳）新能源科技有限公司 | A kind of fire-retardant cellular adaptive temperature control module and preparation method thereof, application |
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Application publication date: 20170329 |