CN106632910A - Preparation method and application of nano aluminum hydroxide graft - Google Patents
Preparation method and application of nano aluminum hydroxide graft Download PDFInfo
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- CN106632910A CN106632910A CN201610921322.9A CN201610921322A CN106632910A CN 106632910 A CN106632910 A CN 106632910A CN 201610921322 A CN201610921322 A CN 201610921322A CN 106632910 A CN106632910 A CN 106632910A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F292/00—Macromolecular compounds obtained by polymerising monomers on to inorganic materials
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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
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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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
- C08L25/00—Compositions of, homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Compositions of derivatives of such polymers
- C08L25/02—Homopolymers or copolymers of hydrocarbons
- C08L25/04—Homopolymers or copolymers of styrene
- C08L25/06—Polystyrene
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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
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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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
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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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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Abstract
The invention relates to a preparation method and application of a nano aluminum hydroxide graft. The preparation method includes the steps of firstly, weighing methyl methacrylate, nano aluminum hydroxide, sodium persulfate, ferric trichloride and sodium dodecyl benzene sulfonate; secondly, mixing the sodium persulfate, the sodium dodecyl benzene sulfonate, the methyl methacrylate and the nano aluminum hydroxide, performing reaction in oil bath of 160-180 DEG C for 6-12 hours, adding the ferric trichloride for demulsification for 6-10 hours, and filtering and washing to obtain the nano aluminum hydroxide graft. The nano aluminum hydroxide graft can be used as the fire retardant applying to polyolefin. The preparation method has the advantages that PMMA is grafted to the nano aluminum hydroxide to form a coating layer on the surface of the nano aluminum hydroxide, the surface energy of nano aluminum hydroxide particles is lowered, the dispersing of the nano aluminum hydroxide in a polyolefin matrix is facilitated, agglomeration of the nano aluminum hydroxide is prevented, and the flame retardance and physical performance of polyolefin composite materials are increased.
Description
Technical field
The invention belongs to technical field of polymer materials, particularly relates to a kind of preparation method of nano-aluminum hydroxide graft
And its application.
Background technology
Nano-aluminum hydroxide has widely been applied in polyolefin flame-retardant material.But the fire retardant polyolefin material of synthesis
Often physical property is bad for material, and anti-wear performance is poor, and nano-aluminum hydroxide Jing often also occurs the phenomenon of reunion.
Given this reason, polymethyl methacrylate (PMMA) nano-aluminum hydroxide is grafted to, then uses its modified polyolefin
Hydrocarbon, it is better than the physical property with the direct improved polyalkene of nano-aluminum hydroxide, anti-flammability, wearability, and pertinent literature is not
See report.
The content of the invention
It is an object of the invention to provide a kind of preparation method and applications of nano-aluminum hydroxide graft, to solve nanometer
The not good problem of physical property of the aluminium hydroxide as fire retardant in polyolefin.
The present invention is achieved by the following technical solutions：
A kind of preparation method of nano-aluminum hydroxide graft, comprises the following steps：
1) methyl methacrylate, nano-aluminum hydroxide, sodium peroxydisulfate, ferric trichloride and DBSA are weighed
Sodium；
2) by the sodium peroxydisulfate, the neopelex, the methyl methacrylate, the nanometer hydrogen-oxygen
Change aluminium mixing, in 160-180 DEG C of oil bath 6-12h is reacted, then add ferric trichloride breakdown of emulsion 6-10h, filtration washing was both obtained
Nano-aluminum hydroxide graft.
A diameter of 60-100nm of the nano-aluminum hydroxide.
The methyl methacrylate, the nano-aluminum hydroxide, the sodium peroxydisulfate, the ferric trichloride and described ten
The mass ratio of dialkyl benzene sulfonic acids sodium is 20-30：40-50：0.2-0.4：1-3：0.1-0.3.
A kind of application of nano-aluminum hydroxide graft, the nano-aluminum hydroxide graft described in any of the above-described is used as resistance
Combustion agent is used in polyolefin.
The polyolefin is in polyethylene, polypropylene, polybutylene terephthalate (PBT), polyamide 6 and polystyrene
One or more of combination.
The invention has the beneficial effects as follows：
The technical program is formed on nano-aluminum hydroxide surface and coated by being grafted PMMA on nano-aluminum hydroxide
Layer, reduces the surface energy of nano-aluminum hydroxide particle, is conducive to dispersion of the nano-aluminum hydroxide in polyolefin substrate, prevents it
Reunion, improve composite polyolefine material anti-flammability and material physical property.
PMMA engrafted nanometer aluminium hydroxides are conducive to improving the interfacial adhesion of nano-aluminum hydroxide and polyolefin substrate, its meeting
The interface transition layer of modulus gradient is formed, the transmission of stress is more beneficial for, this is conducive to improving the physical property of material.
PMMA hardness itself is higher, and its presence improves the crocking resistance of composite polyolefine material.
Specific embodiment
By the following examples describing technical scheme in detail, below example be only it is exemplary, only
Can be used for explaining and illustrating technical scheme, and be not to be construed as the restriction to technical solution of the present invention.
The application provides a kind of preparation method of nano-aluminum hydroxide graft, comprises the following steps：
1) methyl methacrylate (MMA), nano-aluminum hydroxide, sodium peroxydisulfate, ferric trichloride and detergent alkylate are weighed
Sodium sulfonate；
2) by the sodium peroxydisulfate, the neopelex, the methyl methacrylate, the nanometer hydrogen-oxygen
Change aluminium mixing to put into there-necked flask, in 160-180 DEG C of oil bath 6-12h is reacted, then add ferric trichloride breakdown of emulsion 6-
10h, filtration washing had both obtained nano-aluminum hydroxide graft.
A diameter of 60-100nm of the nano-aluminum hydroxide.
The methyl methacrylate, the nano-aluminum hydroxide, the sodium peroxydisulfate, the ferric trichloride and described ten
The mass ratio of dialkyl benzene sulfonic acids sodium is 20-30：40-50：0.2-0.4：1-3：0.1-0.3.
A kind of application of nano-aluminum hydroxide graft, the nano-aluminum hydroxide graft described in any of the above-described is used as resistance
Combustion agent is used in polyolefin.
The polyolefin is polyethylene (PE), polypropylene (PP), polybutylene terephthalate (PBT) (PBT), polyamide 6
(PA6) combination of one or more and in polystyrene (PS).
Raw material used is as follows in embodiments of the invention：
PBT (model 2002U), Polyplastics；PP (model Z30S), Maoming Petrochemical；PE (model 5070), Panjin ethene；
PA6 (model C M1017), toray；PS (model 350), Taiwan state is tall；MMA, the limited public affairs of Chinese medicines group Solution on Chemical Reagents in Shanghai
Department；Neopelex, the triumphant letter chemical industry in Jinan；Sodium peroxydisulfate, Jinan Feng Le chemical industry；Ferric trichloride, the environmental protection of Hubei flourishing age
Science and technology.
Tester used by the present invention is as follows：
ZSK30 type double screw extruders, German W＆P companies；JL-1000 type tensile testing machines, the wide just experiment instrument in Guangzhou
Device company produces；HTL900-T-5B type injection (mo(u)lding) machines, the production of Hai Tai plastics machineries Co., Ltd；XCJ-500 type shock-testings
Machine, the production of Chengde testing machine factory；QT-1196 type tester for elongation, Dongguan City Gao Tai detecting instruments Co., Ltd；QD-GJS-
B12K type homogenizers, Beijing perseverance Order instrument and meter Co., Ltd.
Embodiment 1
1) 2kg methyl methacrylates (MMA), 4kg nano-aluminum hydroxides, 20g sodium peroxydisulfates, 100g tri-chlorinations are weighed
Iron, 10g neopelexes.
2) sodium peroxydisulfate, neopelex, MMA, nano-aluminum hydroxide are put into there-necked flask, 160
DEG C oil bath reaction 6h, then add ferric trichloride breakdown of emulsion 6h, filtration washing both product P1.
Application examples 1
Take 20 parts of P1 to be added in 80 parts of polypropylene (PP), Jing high mixers stirring 10min is subsequently added into double screw extruder
In carry out blending extrusion, obtain PP composite X1.
Wherein, double screw extruder includes six humidity provinces sequentially arranged, and the temperature of the first humidity province is 170 DEG C, the
The temperature of two humidity provinces is 200 DEG C, and the temperature of the 3rd humidity province is 200 DEG C, and the temperature of the 4th humidity province is 200 DEG C, and the 5th is warm
The temperature in degree area is 200 DEG C, and the temperature of the 6th humidity province is 200 DEG C, and the head temperature of double screw extruder is 200 DEG C, screw rod
Rotating speed is 220r/min.
Comparative example 1
Take 20 parts of nano-aluminum hydroxides to be added in 80 parts of polypropylene (PP), Jing high mixers stirring 10min is subsequently added into double
Blending extrusion is carried out in screw extruder, nano-aluminum hydroxide/PP composite D1 are obtained.
PP composites prepared by above-mentioned application examples 1 and comparative example 1 are made into batten with injection machine, its properties of product data
It is as shown in the table:
As can be seen from the above table：
Physical property, anti-wear performance, the fire resistance of X1 is good than D1, and this explanation adds the modified of present invention synthesis
Nano-aluminum hydroxide MODIFIED PP adds the combination property of nano-aluminum hydroxide good than simple.
Embodiment 2
1) 3kg methyl methacrylates (MMA), 5kg nano-aluminum hydroxides, 40g sodium peroxydisulfates, 300g tri-chlorinations are weighed
Iron, 30g neopelexes.
2) sodium peroxydisulfate, neopelex, MMA, nano-aluminum hydroxide are put into there-necked flask, 180
DEG C oil bath reaction 12h, then add ferric trichloride breakdown of emulsion 10h, filtration washing both product P2.
Application examples 2
Take 20 parts of P2 to be added in 80 parts of polybutylene terephthalate (PBT)s (PBT), Jing high mixers stirring 10min, then
Adding in double screw extruder carries out blending extrusion, obtains PBT composite X2.
Wherein, double screw extruder includes six humidity provinces sequentially arranged, and the temperature of the first humidity province is 200 DEG C, the
The temperature of two humidity provinces is 230 DEG C, and the temperature of the 3rd humidity province is 230 DEG C, and the temperature of the 4th humidity province is 230 DEG C, and the 5th is warm
The temperature in degree area is 230 DEG C, and the temperature of the 6th humidity province is 230 DEG C, and the head temperature of double screw extruder is 230 DEG C, screw rod
Rotating speed is 280r/min.
Comparative example 2
Take 20 parts of nano-aluminum hydroxides to be added in 80 parts of PBT, Jing high mixers stirring 10min is subsequently added into twin-screw and squeezes
Going out in machine carries out blending extrusion, obtains nano-aluminum hydroxide/PBT composite D2.
PBT composite prepared by above-mentioned application examples 2 and comparative example 2 is made into batten with injection machine, its properties of product number
According to as shown in the table:
As can be seen from the above table：
Physical property, anti-wear performance, the fire resistance of X2 is good than D2, and this explanation adds the modified of present invention synthesis
Nano-aluminum hydroxide modified PBT adds the combination property of nano-aluminum hydroxide good than simple.
Embodiment 3
1) 2.5kg methyl methacrylates (MMA), 4.5kg nano-aluminum hydroxides, 30g sodium peroxydisulfates, 200g trichlorines are weighed
Change iron, 20g neopelexes.
2) sodium peroxydisulfate, neopelex, MMA, nano-aluminum hydroxide are put into there-necked flask, 170
DEG C oil bath reaction 9h, then add ferric trichloride breakdown of emulsion 8h, filtration washing both product P3.
Application examples 3
Take 20 parts of P3 to be added in 80 parts of polyethylene (PE), Jing high mixers stirring 10min is subsequently added into double screw extruder
In carry out blending extrusion, obtain PE composite X3.
Wherein, double screw extruder includes six humidity provinces sequentially arranged, and the temperature of the first humidity province is 120 DEG C, the
The temperature of two humidity provinces is 170 DEG C, and the temperature of the 3rd humidity province is 170 DEG C, and the temperature of the 4th humidity province is 170 DEG C, and the 5th is warm
The temperature in degree area is 170 DEG C, and the temperature of the 6th humidity province is 170 DEG C, and the head temperature of double screw extruder is 170 DEG C, screw rod
Rotating speed is 260r/min.
Comparative example 3
Take 20 parts of nano-aluminum hydroxides to be added in 80 parts of PE, Jing high mixers stirring 10min is subsequently added into twin-screw extrusion
Blending extrusion is carried out in machine, nano-aluminum hydroxide/PE composite D3 are obtained.
PE composites prepared by above-mentioned application examples 3 and comparative example 3 are made into batten with injection machine, its properties of product data
It is as shown in the table:
As can be seen from the above table：
Physical property, anti-wear performance, the fire resistance of X3 is good than D3, and this explanation adds the modified of present invention synthesis
Nano-aluminum hydroxide modified PE adds the combination property of nano-aluminum hydroxide good than simple.
Embodiment 4
1) 2kg methyl methacrylates (MMA), 4.2kg nano-aluminum hydroxides, 30g sodium peroxydisulfates, 350g tri-chlorinations are weighed
Iron, 20g neopelexes.
2) sodium peroxydisulfate, neopelex, MMA, nano-aluminum hydroxide are put into there-necked flask, 160
DEG C oil bath reaction 8h, then add ferric trichloride breakdown of emulsion 7h, filtration washing both product P4.
Application examples 4
Take 20 parts of P3 to be added in 80 parts of polyamide 6s (PA6), Jing high mixers stirring 10min is subsequently added into twin-screw extrusion
Blending extrusion is carried out in machine, PA6 composite X4 are obtained.
Wherein, double screw extruder includes six humidity provinces sequentially arranged, and the temperature of the first humidity province is 230 DEG C, the
The temperature of two humidity provinces is 240 DEG C, and the temperature of the 3rd humidity province is 240 DEG C, and the temperature of the 4th humidity province is 240 DEG C, and the 5th is warm
The temperature in degree area is 240 DEG C, and the temperature of the 6th humidity province is 240 DEG C, and the head temperature of double screw extruder is 240 DEG C, screw rod
Rotating speed is 320r/min.
Comparative example 4
Take 20 parts of nano-aluminum hydroxides to be added in 80 parts of PA6, Jing high mixers stirring 10min is subsequently added into twin-screw and squeezes
Going out in machine carries out blending extrusion, obtains nano-aluminum hydroxide/PA6 composite D4.
PA6 composites prepared by above-mentioned application examples 4 and comparative example 4 are made into batten with injection machine, its properties of product number
According to as shown in the table:
As can be seen from the above table：
Physical property, anti-wear performance, the fire resistance of X4 is good than D4, and this explanation adds the modified of present invention synthesis
Nano-aluminum hydroxide modified Pa 6 adds the combination property of nano-aluminum hydroxide good than simple.
Embodiment 5
1) 2.2kg methyl methacrylates (MMA), 4.5kg nano-aluminum hydroxides, 35g sodium peroxydisulfates, 280g trichlorines are weighed
Change iron, 30g neopelexes.
2) sodium peroxydisulfate, neopelex, MMA, nano-aluminum hydroxide are put into there-necked flask, 165
DEG C oil bath reaction 9h, then add ferric trichloride breakdown of emulsion 8h, filtration washing both product P5.
Application examples 5
Take 20 parts of P5 to be added in 80 parts of styrene (PS), Jing high mixers stirring 10min is subsequently added into double screw extruder
In carry out blending extrusion, obtain PS composite X5.
Wherein, double screw extruder includes six humidity provinces sequentially arranged, and the temperature of the first humidity province is 160 DEG C, the
The temperature of two humidity provinces is 200 DEG C, and the temperature of the 3rd humidity province is 200 DEG C, and the temperature of the 4th humidity province is 200 DEG C, and the 5th is warm
The temperature in degree area is 200 DEG C, and the temperature of the 6th humidity province is 200 DEG C, and the head temperature of double screw extruder is 200 DEG C, screw rod
Rotating speed is 280r/min.
Comparative example 5
Take 20 parts of nano-aluminum hydroxides to be added in 80 parts of PS, Jing high mixers stirring 10min is subsequently added into twin-screw extrusion
Blending extrusion is carried out in machine, nano-aluminum hydroxide/PS composite D5 are obtained.
PS composites prepared by above-mentioned application examples 5 and comparative example 5 are made into batten with injection machine, its properties of product data
It is as shown in the table:
As can be seen from the above table：
Physical property, anti-wear performance, the fire resistance of X5 is good than D5, and this explanation adds the modified of present invention synthesis
The modified PS of nano-aluminum hydroxide adds the combination property of nano-aluminum hydroxide good than simple.
This patent describes a kind of preparation method of nano-aluminum hydroxide graft, and obtained polyolefine material is in thing
Reason aspect of performance is also improved to some extent, and this greatly expands the application of composite polyolefine material, with weighing very much
The meaning wanted.
The above is only the description of the preferred embodiment of the present invention, it is noted that due to the finiteness of literal expression, and
Objectively there is unlimited concrete structure, for those skilled in the art, without departing from the principle of the invention
On the premise of, some improvements and modifications can also be made, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (5)
1. a kind of preparation method of nano-aluminum hydroxide graft, it is characterised in that：Comprise the following steps：
1) methyl methacrylate, nano-aluminum hydroxide, sodium peroxydisulfate, ferric trichloride and neopelex are weighed；
2) by the sodium peroxydisulfate, the neopelex, the methyl methacrylate, the nano-aluminum hydroxide
Mixing, in 160-180 DEG C of oil bath 6-12h is reacted, and then adds ferric trichloride breakdown of emulsion 6-10h, and filtration washing had both obtained nanometer
Aluminium hydroxide graft.
2. the preparation method of nano-aluminum hydroxide graft according to claim 1, it is characterised in that：The nanometer hydrogen-oxygen
Change a diameter of 60-100nm of aluminium.
3. the preparation method of nano-aluminum hydroxide graft according to claim 1, it is characterised in that：The metering system
The quality of sour methyl esters, the nano-aluminum hydroxide, the sodium peroxydisulfate, the ferric trichloride and the neopelex
Than for 20-30：40-50：0.2-0.4：1-3：0.1-0.3.
4. a kind of application of nano-aluminum hydroxide graft, it is characterised in that：Any one of the claims 1 to 3
Nano-aluminum hydroxide graft is used in polyolefin as fire retardant.
5. the application of nano-aluminum hydroxide graft according to claim 4, it is characterised in that：The polyolefin is poly- second
The combination of one or more in alkene, polypropylene, polybutylene terephthalate (PBT), polyamide 6 and polystyrene.
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Cited By (3)
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| CN107417974A (en) * | 2017-06-21 | 2017-12-01 | 安徽江淮汽车集团股份有限公司 | A kind of modified micaceous powder and preparation method thereof |
| CN114590852A (en) * | 2022-03-31 | 2022-06-07 | 高点(深圳)科技有限公司 | Hydroxide grafted oxide type positive electrode material precursor and preparation method and application thereof |
| CN117964962A (en) * | 2024-03-29 | 2024-05-03 | 瑞淙生物科技(山东)有限责任公司 | High-temperature-resistant high-molecular profile and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107417974A (en) * | 2017-06-21 | 2017-12-01 | 安徽江淮汽车集团股份有限公司 | A kind of modified micaceous powder and preparation method thereof |
| CN114590852A (en) * | 2022-03-31 | 2022-06-07 | 高点(深圳)科技有限公司 | Hydroxide grafted oxide type positive electrode material precursor and preparation method and application thereof |
| CN114590852B (en) * | 2022-03-31 | 2024-04-02 | 高点(深圳)科技有限公司 | Hydroxide grafted oxide type positive electrode material precursor, and preparation method and application thereof |
| CN117964962A (en) * | 2024-03-29 | 2024-05-03 | 瑞淙生物科技(山东)有限责任公司 | High-temperature-resistant high-molecular profile and preparation method thereof |
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