CN106543632A - A kind of load TiO2Diatomaceous flame retardant automotive plastic uptake material and preparation method thereof - Google Patents
A kind of load TiO2Diatomaceous flame retardant automotive plastic uptake material and preparation method thereof Download PDFInfo
- Publication number
- CN106543632A CN106543632A CN201610937417.XA CN201610937417A CN106543632A CN 106543632 A CN106543632 A CN 106543632A CN 201610937417 A CN201610937417 A CN 201610937417A CN 106543632 A CN106543632 A CN 106543632A
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- resin
- flame retardant
- abs
- plastic uptake
- diatomaceous
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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
-
- 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
-
- 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
-
- 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
-
- 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
Abstract
The invention discloses a kind of load TiO2Diatomaceous flame retardant automotive plastic uptake material, 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, butyl titanate, glacial acetic acid, nitric acid, diatomite, cerous nitrate etc. be raw material.Intermediary's porous molecular sieve of the present invention produces bonded effect with linear phenolic resin, improves matrix resin heat endurance；Microencapsulation 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 endurance of resin, and mechanical property is also higher；Obtain a kind of load TiO2Diatomaceous flame retardant automotive plastic uptake material.
Description
Technical field
The present invention relates to the field of fire-proof technology of composite, and in particular to a kind of load TiO2- diatomaceous fire-retardant vapour
Car 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 ABS matrix compatibilities
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 endurance is improve；With in-situ polymerization
Method is prepared for microencapsulation APP, is prepared for Ultrafine Antimony-Oxide/Kaolin Composite Powder with ball-milling method, and Graphene is added to
In ABS resin matrix, hence it is evident that improve the anti-flammability and heat endurance of resin, mechanical property is also higher；Finally obtain a kind of negative
Carry TiO2- diatomaceous flame retardant automotive plastic uptake material.
The content of the invention
The invention mainly solves the technical problem of providing a kind of load TiO2- diatomaceous flame retardant automotive 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, the table of ultra-hydrophobicity
The characteristic such as surface self-cleaning effect and self-cleaning.
The technical problem to be solved is realized using following technical scheme：
Acrylonitrile-butadiene-styrene copolymer (ABS) 43-50, linear phenol-aldehyde resin 3-9, microcapsule red phosphorus 5-8, alkali formula
Magnesium sulfate crystal whisker 2-5, nitrile rubber 3-5, mesoporous molecular sieve SBA-15 4-10, APP 5-9, melamine resin
2-5, kaolin 1-3, Sb2O33-8, dimethicone 1-3, Graphene 3-8, butyl titanate 2-5, glacial acetic acid 0.2-0.5, nitric acid
0.1-0.3, diatomite 1-3, cerous nitrate 1-2, ethanol, distilled water, acetic acid, Sodium hydroxide q. s.
A kind of load TiO2The preparation method of-diatomaceous flame retardant automotive plastic uptake material, it is characterised in that according to the following steps
Carry out：
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 absolute ethyl 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, suction 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
Slurries, are put into baking oven after ball milling 4-6h, in 110-130 DEG C of drying 5-8h, obtain composite micro-powder, and which is mixed with resulting material in b
Uniformly, add dimethicone at 60-120 DEG C, whip modified 15-60min, suction 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. in butyl titanate 1:2-3 adds absolute ethyl alcohol, adds glacial acetic acid, nitric acid, stirs 1-2h, forms solution A；To
Add water to stir into suspension in diatomite, add nitrate, NaOH ethanol solution, mixing and stirring to be formed and suspended
Liquid B；B is slowly added in A, and with stirring 0.5-1h, still aging 1-2h forms gel, 1- is dried in 100-130 DEG C
2h, then Jing 580-650 DEG C heat treatment insulation 3-5h, obtain TiO2/ diatomite composite photocatalytic material；
F. resulting material in c, d, e and other residual components are blended at 185-195 DEG C, discharge and place after mixing is uniform
In mould, the hot pressing 10-30min on 180-190 DEG C of the vulcanizing press, then the 10-30min that colds pressing at room temperature, go out molding
The ABS plastic sheet material that must be modified, that is, obtain a kind of load TiO2- diatomaceous flame retardant automotive 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 endurance.
（2）Microencapsulation 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 synergy well 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 micro mist, 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 endurance of resin, mechanical property is also higher.
（5）TiO2- diatomite composite photocatalytic material itself possesses photodegradation, and composite has ultra-hydrophobicity
Clean surfaces net effect and the characteristic such as self-cleaning, present invention process is simple, easy to operate, invests little, and operating cost is low, to ring
Border is pollution-free.
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
A kind of load TiO2- diatomaceous flame retardant automotive plastic uptake material, is obtained by the raw material of following weight parts (g)：
Acrylonitrile-butadiene-styrene copolymer (ABS) 44, linear phenol-aldehyde resin 9, microcapsule red phosphorus 8, alkali magnesium sulfate are brilliant
Palpus 2, nitrile rubber 3, mesoporous molecular sieve SBA-15 4, APP 5, melamine resin 2, kaolin 1, Sb2O33, two
Methyl-silicone oil 1, Graphene 3, butyl titanate 2, glacial acetic acid 0.2, nitric acid 0.1, diatomite 3, cerous nitrate 1, ethanol, distilled water, second
Acid, Sodium hydroxide q. s.
A kind of load TiO2The preparation method of-diatomaceous flame retardant automotive plastic uptake material, it is characterised in that according to the following steps
Carry out：
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 absolute ethyl 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, suction filtration, washing, dry the microencapsulation 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 slurries,
Baking oven is put into after ball milling 4h, in 130 DEG C of dryings 5h, composite micro-powder is obtained, which is well mixed with resulting material in b, at 80 DEG C
Add dimethicone, whip modified 30min, suction 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. in butyl titanate 1:2 add absolute ethyl alcohol, add glacial acetic acid, nitric acid, stir 1h, form solution A；To diatom
Add water to stir into suspension in soil, add nitrate, NaOH ethanol solution, mixing and stirring to form suspension B；
B is slowly added in A, and with stirring 1h, still aging 1h forms gel, 2h, then Jing 600- are dried in 120-130 DEG C
620 DEG C of heat treatment insulation 3h, obtain TiO2/ diatomite composite photocatalytic material；
F. resulting material in c, d, e and other residual components are blended at 185-195 DEG C, discharge and place after mixing is uniform
In mould, the hot pressing 30min on 180-190 DEG C of the vulcanizing press, then the 30min that colds pressing at room temperature, depanning is obtained modified
ABS plastic sheet material, that is, obtain a kind of load TiO2- diatomaceous flame retardant automotive plastic uptake material.
A kind of load TiO prepared by above-described embodiment2The performance test results of-diatomaceous flame retardant automotive plastic uptake material are such as
Shown in lower：
Up to UL-94 V-0 levels, LOI values 29%, carbon yield (600 DEG C) 18%, tensile strength reaches the vertical combustion performance of flame-proof ABS
47MPa, notch impact strength are 28 KJ/m2, elongation at break 39%.
Claims (2)
1. it is a kind of to load TiO2- diatomaceous flame retardant automotive plastic uptake material, it is characterised in that be obtained by the raw material of following weight parts：
Acrylonitrile-butadiene-styrene copolymer (ABS) 43-50, linear phenol-aldehyde resin 3-9, microcapsule red phosphorus 5-8, alkali formula
Magnesium sulfate crystal whisker 2-5, nitrile rubber 3-5, mesoporous molecular sieve SBA-15 4-10, APP 5-9, melamine resin
2-5, kaolin 1-3, Sb2O33-8, dimethicone 1-3, Graphene 3-8, butyl titanate 2-5, glacial acetic acid 0.2-0.5, nitric acid
0.1-0.3, diatomite 1-3, cerous nitrate 1-2, ethanol, distilled water, acetic acid, Sodium hydroxide q. s.
2. one kind according to claim 1 loads TiO2The preparation method of-diatomaceous flame retardant automotive plastic uptake material, which is special
Levy and be, 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 microcapsules red
Phosphorus, continues reaction 1-2h, product is placed in absolute ethyl 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, suction 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
Slurries, are put into baking oven after ball milling 4-6h, in 110-130 DEG C of drying 5-8h, obtain composite micro-powder, and which is mixed with resulting material in b
Uniformly, add dimethicone at 60-120 DEG C, whip modified 15-60min, suction 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. in butyl titanate 1:2-3 adds absolute ethyl alcohol, adds glacial acetic acid, nitric acid, stirs 1-2h, forms solution A；To
Add water to stir into suspension in diatomite, add nitrate, NaOH ethanol solution, mixing and stirring to be formed and suspended
Liquid B；B is slowly added in A, and with stirring 0.5-1h, still aging 1-2h forms gel, 1- is dried in 100-130 DEG C
2h, then Jing 580-650 DEG C heat treatment insulation 3-5h, obtain TiO2/ diatomite composite photocatalytic material；
F. resulting material in c, d, e and other residual components are blended at 185-195 DEG C, discharge and place after mixing is uniform
In mould, the hot pressing 10-30min on 180-190 DEG C of the vulcanizing press, then the 10-30min that colds pressing at room temperature, go out molding
The ABS plastic sheet material that must be modified, that is, obtain a kind of load TiO2- diatomaceous flame retardant automotive plastic uptake material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110396328A (en) * | 2019-07-16 | 2019-11-01 | 河北工业大学 | A kind of preparation method of liquid rubber removing graphene and its super-hydrophobic composite material |
| CN115896967A (en) * | 2022-12-13 | 2023-04-04 | 泰安亚荣生物科技有限公司 | Degradable environment-friendly flame retardant and preparation method thereof |
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| CN104046014A (en) * | 2014-05-19 | 2014-09-17 | 安徽安缆模具有限公司 | Halogen-free flame-retardant automobile nylon composite and preparation method thereof |
| CN104194077A (en) * | 2014-09-22 | 2014-12-10 | 安徽电气集团股份有限公司 | Anti-abrasion and flame-retardant modified natural rubber |
| CN104629158A (en) * | 2015-01-29 | 2015-05-20 | 安徽万泰电缆有限公司 | Modified mining cable sheathing material |
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| CN103122097A (en) * | 2013-01-22 | 2013-05-29 | 安徽华津电缆集团有限公司 | Thermoplastic low-smoke halogen-free flame-retardant environment-friendly sheath material for power cables and preparation method thereof |
| CN104046014A (en) * | 2014-05-19 | 2014-09-17 | 安徽安缆模具有限公司 | Halogen-free flame-retardant automobile nylon composite and preparation method thereof |
| CN104194077A (en) * | 2014-09-22 | 2014-12-10 | 安徽电气集团股份有限公司 | Anti-abrasion and flame-retardant modified natural rubber |
| CN104629158A (en) * | 2015-01-29 | 2015-05-20 | 安徽万泰电缆有限公司 | Modified mining cable sheathing material |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110396328A (en) * | 2019-07-16 | 2019-11-01 | 河北工业大学 | A kind of preparation method of liquid rubber removing graphene and its super-hydrophobic composite material |
| CN110396328B (en) * | 2019-07-16 | 2020-12-25 | 河北工业大学 | Preparation method of liquid rubber-stripped graphene and super-hydrophobic composite material thereof |
| CN115896967A (en) * | 2022-12-13 | 2023-04-04 | 泰安亚荣生物科技有限公司 | Degradable environment-friendly flame retardant and preparation method thereof |
| CN115896967B (en) * | 2022-12-13 | 2023-06-13 | 泰安亚荣生物科技有限公司 | Degradable environment-friendly flame retardant and preparation method thereof |
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Application publication date: 20170329 |