CN109880160A - A kind of aluminium hydroxide and montmorillonite nano composite flame-proof agent and preparation method thereof - Google Patents
A kind of aluminium hydroxide and montmorillonite nano composite flame-proof agent and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of aluminium hydroxides and montmorillonite nano composite flame-proof agent and preparation method thereof, belong to technical field of nano material.Aluminium hydroxide and montmorillonite nano composite flame-proof agent of the invention, is to be prepared by aluminium hydroxide and montmorillonite with mechanochemical reaction；During aluminium hydroxide and montmorillonite mixing and ball milling, form stable aluminium hydroxide-montmorillonite Composite particle, the montmorillonite layer being stripped is attached on aluminum hydroxide particles surface, so that montmorillonite is evenly dispersed with the lamellar structure of nanoscale in aluminium hydroxide powder, it avoids montmorillonite layer from stacking again, lays the foundation for further application and the preparation of polymer nanocomposite composite flame-retardant agent of fire retardant in the polymer.
Description
Technical field
The present invention relates to a kind of aluminium hydroxides and montmorillonite nano composite flame-proof agent and preparation method thereof, belong to nano material
Technical field.
Background technique
Montmorillonite (montmorillonite, MMT) is a kind of typical nano layered silicate, and reserves are big, are applied to
This is low, and has nano-meter characteristic, is therefore widely used in every field.It polymerize when montmorillonite is prepared with polymer
When object/Nano composite material of montmorillonite, mechanical performance, the makings barrier property, flame retardant property of composite material can be improved, however
The only above-mentioned beneficial effect of competence exertion when montmorillonite reaches the fine dispersion of nanoscale in the polymer.Between cheating engaging layer
A large amount of inorganic cations appear as hydrophilic and oleophobic property, are difficult to reach ideal dispersion effect in a polymer matrix, usually
Solution be organically-modified processing, but organic montmorillonite can not neglect the negative effect of the fire-retardant performance of composite material sometimes
Depending on.
Although the thermal stability of nano composite polymer-montmorillonoid material, at charcoal be improved significantly, self-extinguishment
Property it is still poor, ideal UL-94 burning rank cannot be reached, therefore at present for nano composite polymer-montmorillonoid material
Research all stress for montmorillonite and other fire retardants to be used in compounding, to reach better flame retardant effect.
Aluminium hydroxide (Aluminium hydroxide, ATH) is typical inorganic fill type fire retardant, resourceful, valence
Lattice are cheap, environmental-friendly, and have the effects that fire-retardant, smoke elimination, filling, are widely used in fire proofing.Its fire retardant mechanism is
Cold-trap effect, dilution effect, blocking effect, mechanism determine that its flame retarding efficiency is lower, generally require to reach good effect
Higher loading.To improve its flame retarding efficiency, other than the means such as common ultra fine, organically-modified, usually by hydrogen
Aluminium oxide is used in compounding with synergist.Document " Flame retardancy and thermal stability of
ethylene-vinyl acetate copolymer nanocomposites with alumina trihydrate and
Montmorillonite " in mention aluminium hydroxide and when montmorillonite is used in compounding can further improve ethylene-vinyl acetate
The oxygen index (OI) of copolymer, but it when use is used in compounding, there are still disperse uneven asking in a polymer matrix for montmorillonite
Topic.
Therefore pre-dispersion of the montmorillonite in fire retardant is a spotlight in the prior art, fire-retardant that will compound
System is added before polymer, first montmorillonite is dispersed in fire retardant, so that it can be better dispersed in process
In a polymer matrix.The prior art is broadly divided into two classes based on this laboratory patent applied for: a kind of ammonium polyphosphate and layer
The double hydroxyl hydroxide nanometer complexes of shape and preparation method thereof (application number CN201310235150.6) and a kind of melamine cyanogen
Lithate and montmorillonite nano complex and preparation method thereof (CN201510284785.4) are the first kind, and technical essential is to hinder
Montmorillonite is added in combustion agent synthesis process；A kind of DOPO/MMT composite nanometer flame retardant and preparation method thereof
(CN201610115310.7) it is the second class, uses the montmorillonite of fire retardant intercalation modifying in advance.It is equal that its advantage concentrates on montmorillonite
It can be dispersed in fire retardant in advance, but above-mentioned technology is liquid phase reactor, be related to the taking back and process of solvent, environment is deposited
In potential hazard.
Mechanochemical reaction method be it is a kind of be widely used in inoganic particle modified method, utilize the machinery generated between medium
Physics, the chemical structure of inorganic particulate can be changed.There are many utilize mechanochemical reaction modified aluminium hydroxide or montmorillonite
Method is suggested, such as the method (application number CN201410530193) that ultrafine aluminium hydroxide surface is modified, and a kind of filler grade is high
The production method (application number CN201310162126.4) of white aluminum hydroxide, organic modification method of montmorillonite flame retardant (application number
) and document " Effect of ball milling on the structure of Na CN201110235357.4+-
Montmorillonite and organo-montmorillonite (Cloisite 30B) " in mention mechanochemical reaction can
Keep MMT peeling-off, advantage concentrates on using adjusting diameter of particle or improves organic modification montmonrillonite dispersibility.But individually place
The effect for managing montmorillonite is limited, can not reach complete removing dispersion.Mechanochemical reaction is used still without document report at present
Realize montmorillonite pre-dispersion.
Summary of the invention
A kind of aluminium hydroxide is provided the purpose of the present invention is to solve the problem of existing fire retardant effect difference and is covered
De- soil composite nanometer flame retardant and preparation method thereof.
The purpose of the present invention is what is be achieved through the following technical solutions.
A kind of aluminium hydroxide and montmorillonite nano composite flame-proof agent of the invention, is by aluminium hydroxide and montmorillonite by machinery
Chemical method is prepared, mass percent are as follows: aluminium hydroxide 80%-94%, montmorillonite 6%-20%.
The preparation method of a kind of aluminium hydroxide and montmorillonite nano composite flame-proof agent of the invention, specific preparation step is such as
Under: the aluminium hydroxide is unmodified synthesis aluminium hydroxide
Aluminium hydroxide is dried in an oven with montmorillonite, is placed in ball mill container after mixing；By zirconium oxide ball milling pearl
It is placed in ball mill container, ball milling pearl and powder quality ratio are 1:10~1:20, and ball milling pearl and powder account for ball mill container volume altogether
20%~50%.Be arranged comprehensive ball-milling technology condition: it with 30 °~60 ° is interval revolution that condition 1, which is chassis, after rotation
It maintains 5~50 minutes, maintenance period runs chassis rotation technique；Condition 2 be chassis with 30 °/minute~90 °/minute angle speed
The lasting revolution of degree, during which runs chassis rotation technique；Condition 3 mixes setting with condition 2 for condition 1 in any way.Chassis is certainly
Skill of changing a job is that chassis rotates clockwise 1~4 minute, shuts down 1 minute, rotates 1~4 minute counterclockwise, shuts down 1 minute and follows for one
Ring, revolving speed are 500~800rpm.After comprehensive 1~5h of ball milling, sieving obtains a kind of aluminium hydroxide and the compound resistance of montmorillonite-based nano
Fire agent；
The preparation method of a kind of aluminium hydroxide and montmorillonite nano composite flame-proof agent of the invention, specific preparation step is such as
Under: the aluminium hydroxide is organically-modified aluminium hydroxide.
Aluminium hydroxide is dried in an oven with montmorillonite, and 1 ratio is placed in ball mill container after mixing as required；It will
Zirconium oxide ball milling pearl be placed in ball mill container, ball milling pearl and powder quality ratio are 1:15~1:15, and ball milling pearl and powder account for ball altogether
Grind the 20%~50% of container volume.Be arranged comprehensive ball-milling technology condition: it with 30 °~60 ° is interval public affairs that condition 1, which is chassis,
Turn, maintained 5~50 minutes after rotation, maintenance period runs chassis rotation technique；Condition 2 be chassis with 30 °/minute~
The angular speed of 90 °/minute persistently revolves, and during which runs chassis rotation technique；Condition 3 is that condition 1 is mixed in any way with condition 2
Close setting.Rotation technique in chassis is that chassis rotates clockwise 1~4 minute, shuts down 1 minute, rotates 1~4 minute counterclockwise, shuts down
1 minute is a circulation, and revolving speed is 300~600rpm.After comprehensive 1~5h of ball milling, a kind of aluminium hydroxide is obtained through sieving and is covered
De- soil composite nanometer flame retardant；
Montmorillonite described in above-mentioned steps can be calcium-base montmorillonite, sodium-based montmorillonite and organic modification montmonrillonite, or contain
There is the clay of montmorillonite structure.
Beneficial effect
1, the present invention prepares aluminium hydroxide and montmorillonite nano composite flame-proof agent using ball-milling method, is weakened using mechanical energy and is covered
The interlaminar action power for taking off soil makes montmorillonite layer that sliding gradually occur and removes, while when aluminium hydroxide is by impact force and pressure
Partial size reduces, and the cheating engaging layer and aluminum hydroxide particles removed adsorb to form stable composite nanometer flame retardant.
2, this method simple process, raw material are easy to get, at low cost, are suitble to industrial application, and organic solvent-free is environmental-friendly.With
Comprehensive ball-milling method prepares the composite nanometer flame retardant of aluminium hydroxide and montmorillonite obtained, realizes montmorillonite in aluminium hydroxide
Preparatory dispersion in fire retardant, it is contemplated that the nanometer effect of montmorillonite can be enhanced when being applied in polymer nanocomposites
Answer, to improve flame retardant property and thermal stability, for fire retardant in the polymer further apply and polymer nanocomposite is compound
The preparation of fire retardant lays the foundation.
Detailed description of the invention
Fig. 1 is aluminium hydroxide montmorillonite-based nano prepared by aluminium hydroxide, the XRD spectra of calcium-base montmorillonite and embodiment 1
The XRD spectra of composite flame-retardant agent；
Fig. 2 is that the dispersion of montmorillonite in the aluminium hydroxide montmorillonite nano composite flame-proof agent prepared in embodiment 1 is shown
It is intended to.
Specific embodiment
The present invention will be further described with embodiment with reference to the accompanying drawing, and example is not intended to limit protection model of the invention
It encloses.
Embodiment 1
A kind of aluminium hydroxide and montmorillonite nano composite flame-proof agent of the invention, is by aluminium hydroxide and montmorillonite ball milling system
It is standby to form, mass percent are as follows: unmodified synthesis aluminium hydroxide 88.9%, montmorillonite 11.1%.
The unmodified synthesis aluminium hydroxide of 24.24g is dried in an oven with 3.03g calcium-base montmorillonite (mass ratio 8:1),
It is placed in ball grinder after mixing；272.73g ball milling pearl is placed in ball grinder, control powder and ball milling pearl mass ratio are 1:
10, ball milling pearl and powder account for the 20% of ball mill container volume altogether；Comprehensive ball-milling technology condition is arranged: chassis is with 90 °/minute
Angular speed persistently revolves, and during which runs chassis rotation technique；Rotation technique in chassis is that chassis rotates clockwise 3 minutes, shuts down 1 point
Clock, rotation 3 minutes, shut down 1 minute as a circulation, rotation revolving speed is 700rpm counterclockwise.Sieving obtains hydroxide after ball milling 3h
Aluminium and montmorillonite nano composite flame-proof agent.
From the XRD spectra of montmorillonite it is found that 2 θ=5.88 ° are the characteristic diffraction peak of montmorillonite；From aluminium hydroxide montmorillonite
The XRD spectra of composite nanometer flame retardant shows the stratiform of montmorillonite it is found that the intensity of diffraction maximum is greatly reduced at 2 θ=5.88 °
Structure is destroyed in mechanical milling process, and lamella is peeling-off；It can from the TEM photo of aluminium hydroxide montmorillonite nano composite flame-proof agent
Know, the montmorillonite layer of removing is dispersed in aluminium hydroxide, and substantially uniformity is separated into the lamellar structure of nanoscale.
Embodiment 2
A kind of aluminium hydroxide and montmorillonite nano composite flame-proof agent of the invention, is by aluminium hydroxide and montmorillonite ball milling system
It is standby to form, mass percent are as follows: unmodified synthesis aluminium hydroxide 91.7%, sodium-based montmorillonite 8.3%.
The unmodified synthesis aluminium hydroxide of 28.41g is dried in an oven with 2.84g sodium-based montmorillonite (mass ratio 10:1)
It is dry, it is placed in ball grinder after mixing；468.75g ball milling pearl is placed in ball grinder, powder and ball milling pearl mass ratio are 1:15,
Ball milling pearl and powder account for the 32% of ball mill container volume altogether；Comprehensive ball-milling technology condition is arranged: chassis is public for interval with 45 °
Turn, maintained 6 minutes after rotation, maintenance period runs chassis rotation technique；Rotation technique in chassis is that chassis rotates clockwise 2
Minute, it shuts down 1 minute, counterclockwise rotation 2 minutes, shuts down 1 minute as a circulation, rotation revolving speed is 800rpm.Mistake after ball milling 1h
Sieve obtains aluminium hydroxide and montmorillonite nano composite flame-proof agent.
Embodiment 3
A kind of aluminium hydroxide and montmorillonite nano composite flame-proof agent of the invention, is by aluminium hydroxide and montmorillonite ball milling system
It is standby to form, mass percent are as follows: organically-modified aluminium hydroxide 93.7%, calcium-base montmorillonite 6.3%.
The organically-modified aluminium hydroxide of 46.88g is dried in an oven with 3.13g montmorillonite (mass ratio 15:1), is mixed
Uniform postposition enters ball grinder；250.00g ball milling pearl is placed in ball grinder, powder and ball milling pearl mass ratio are 1:5, ball milling pearl with
Powder accounts for the 20% of ball mill container volume altogether；Be arranged comprehensive ball-milling technology condition: it with 30 ° is interval revolution that condition 1, which is chassis,
It is maintained 10 minutes after rotation, maintenance period runs chassis rotation technique；Condition 2 is that chassis is held with the angular speed of 60 °/minute
Continuous revolution, during which runs chassis rotation technique；Condition 1 is run with condition 2 to replace after twenty minutes.Rotation technique in chassis is chassis
It rotates clockwise 4 minutes, shuts down 1 minute, counterclockwise rotation 4 minutes, shut down 1 minute as a circulation, rotation revolving speed is 500rpm.
Sieving obtains aluminium hydroxide and montmorillonite nano composite flame-proof agent after ball milling 1h.
Embodiment 4
A kind of aluminium hydroxide and montmorillonite nano composite flame-proof agent of the invention, is by aluminium hydroxide and montmorillonite ball milling system
It is standby to form, mass percent are as follows: unmodified synthesis aluminium hydroxide 83.3%, organic modification montmonrillonite 16.7%.
In an oven by the unmodified synthesis aluminium hydroxide of 31.75g and 6.35g organic modification montmonrillonite (mass ratio 5:1)
Drying, is placed in ball grinder after mixing；761.90g ball milling pearl is placed in ball grinder, powder and ball milling pearl mass ratio are 1:
20, ball milling pearl and powder account for the 50% of ball mill container volume altogether；Comprehensive ball-milling technology condition is arranged: chassis is with 45 °/minute
Angular speed persistently revolves, and during which runs chassis rotation technique；Rotation technique in chassis is that chassis rotates clockwise 4 minutes, shuts down 1 point
Clock, rotation 4 minutes, shut down 1 minute as a circulation, rotation revolving speed is 800rpm counterclockwise.Sieving obtains hydroxide after ball milling 5h
Aluminium and montmorillonite nano composite flame-proof agent.
Embodiment 5
A kind of aluminium hydroxide and montmorillonite nano composite flame-proof agent of the invention, is by aluminium hydroxide and montmorillonite ball milling system
It is standby to form, mass percent are as follows: unmodified synthesis aluminium hydroxide 80%, calcium-base montmorillonite 20%.
The unmodified synthesis aluminium hydroxide of 30.00g is dried in an oven with 7.50g calcium-base montmorillonite (mass ratio 4:1),
It is placed in ball grinder after mixing；It is 1:15 that 562.50.00g ball milling pearl, which is placed in powder and ball milling pearl mass ratio in ball grinder,
Ball milling pearl and powder account for the 38% of ball mill container volume altogether；Comprehensive ball-milling technology condition is arranged: chassis is public for interval with 30 °
Turn, maintained 30 minutes after rotation, maintenance period runs chassis rotation technique；Chassis rotation technique rotates clockwise for chassis
It 2 minutes, shuts down 1 minute, counterclockwise rotation 2 minutes, shuts down 1 minute as a circulation, rotation revolving speed is 800rpm.Mistake after ball milling 4h
Sieve obtains aluminium hydroxide and montmorillonite nano composite flame-proof agent.
Embodiment 6
A kind of aluminium hydroxide and montmorillonite nano composite flame-proof agent of the invention, is by aluminium hydroxide and montmorillonite ball milling system
It is standby to form, mass percent are as follows: organically-modified aluminium hydroxide 90%, sodium-based montmorillonite 10%.
The organically-modified aluminium hydroxide of 17.14g is dried in an oven with 1.90g sodium-based montmorillonite (mass ratio 9:1), is mixed
It closes uniform postposition and enters ball grinder；380.95g ball milling pearl is placed in ball grinder, powder and ball milling pearl mass ratio are 1:20, ball milling
Pearl and powder account for the 26% of ball mill container volume altogether；Be arranged comprehensive ball-milling technology condition: it with 60 ° is interval that condition 1, which is chassis,
Revolution, maintains 5 minutes after rotation, and maintenance period runs chassis rotation technique；Condition 2 is chassis with the angle speed of 90 °/minute
The lasting revolution of degree, during which runs chassis rotation technique；Condition 1 replaces after running 30 minutes with condition 2.Chassis rotation technique is
Chassis rotates clockwise 1 minute, shuts down 1 minute, counterclockwise rotation 1 minute, shuts down 1 minute as a circulation, rotation revolving speed is
500rpm.Sieving obtains aluminium hydroxide and montmorillonite nano composite flame-proof agent after ball milling 2h.
For the flame retardant effect for testing each embodiment obtained aluminium hydroxide and Montmorillonite composite fire retardant, by itself and ethylene-
Vinyl acetate co-polymer is prepared into flame retardant composite material, used in fire retardant and ethylene-vinyl acetate copolymer
It is identical in quality, carry out limit oxygen index LOI and UL-94 vertical burn test.
Above-described specific descriptions have carried out further specifically the purpose of invention, technical scheme and beneficial effects
It is bright, it should be understood that the above is only a specific embodiment of the present invention, the protection model being not intended to limit the present invention
It encloses, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should be included in the present invention
Protection scope within.
Claims (6)
1. a kind of aluminium hydroxide and montmorillonite nano composite flame-proof agent, it is characterised in that: be by aluminium hydroxide and montmorillonite by machine
Tool chemical method is prepared, and aluminium hydroxide accounts for the 80%-94% of aluminium hydroxide Yu montmorillonite gross mass.
2. preparing a kind of method of aluminium hydroxide and montmorillonite nano composite flame-proof agent as described in claim 1, feature exists
In: specific step is as follows: the aluminium hydroxide is unmodified synthesis aluminium hydroxide；
Aluminium hydroxide is dried in an oven with montmorillonite, is placed in ball mill container after mixing；Zirconium oxide ball milling pearl is placed in
Ball mill container, ball milling pearl and powder quality ratio are 1:10~1:20, ball milling pearl and powder account for altogether ball mill container volume 20%~
50%；Comprehensive ball-milling technology condition is set, and the comprehensive ball-milling technology condition is divided into any one in three conditions；Item
It is interval revolution that part 1, which is chassis with 30 °~60 °, is maintained 5~50 minutes after rotation, maintenance period operation chassis oneself change a job
Skill；Condition 2 be chassis with 30 °/minute~90 °/minute angular speed persistently revolve, during which run chassis rotation technique；Condition 3
Setting is mixed in any way with condition 2 for condition 1；After comprehensive 1~5h of ball milling, sieving obtains a kind of aluminium hydroxide and covers de-
Native composite nanometer flame retardant.
3. preparing a kind of method of aluminium hydroxide and montmorillonite nano composite flame-proof agent as described in claim 1, feature exists
In: specific step is as follows: the aluminium hydroxide is organically-modified aluminium hydroxide；
Aluminium hydroxide is dried in an oven with montmorillonite, is placed in ball mill container after mixing；Zirconium oxide ball milling pearl is placed in
Ball mill container, ball milling pearl and powder quality ratio are 1:15~1:15, ball milling pearl and powder account for altogether ball mill container volume 20%~
50%；Comprehensive ball-milling technology condition is set, and the comprehensive ball-milling technology condition is divided into any one in three conditions；Item
It is interval revolution that part 1, which is chassis with 30 °~60 °, is maintained 5~50 minutes after rotation, maintenance period operation chassis oneself change a job
Skill；Condition 2 be chassis with 30 °/minute~90 °/minute angular speed persistently revolve, during which run chassis rotation technique；Condition 3
Setting is mixed in any way with condition 2 for condition 1；After comprehensive 1~5h of ball milling, a kind of aluminium hydroxide is obtained through sieving and is covered
De- soil composite nanometer flame retardant.
4. method according to claim 2, it is characterised in that: the chassis rotation technique is that chassis rotates clockwise 1~4 point
Clock is shut down 1 minute, and another mistake hour hands rotate 1~4 minute, is shut down 1 minute, is recycled as one, and revolving speed is 500~800rpm.
5. method as claimed in claim 3, it is characterised in that: rotation technique in chassis is that chassis rotates clockwise 1~4 minute,
It shuts down 1 minute, rotates 1~4 minute counterclockwise, shut down 1 minute, recycled as one, revolving speed is 300~600rpm.
6. method as claimed in claim 2 or claim 3, it is characterised in that: montmorillonite described in above-mentioned steps includes: calcium Ji Mengtuo
Soil, sodium-based montmorillonite, organic modification montmonrillonite or the clay containing montmorillonite structure.
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| CN201910158980.0A CN109880160B (en) | 2019-03-04 | 2019-03-04 | Aluminum hydroxide and montmorillonite nano composite flame retardant and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111808798A (en) * | 2020-09-03 | 2020-10-23 | 朗姿赛尔生物科技（广州）有限公司 | Culture medium for promoting stem cell expansion |
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| CN1752130A (en) * | 2004-09-22 | 2006-03-29 | 北京化工大学 | Fire retardant composite material of nano-aluminium hydroxide, clay and ethylene-vinyl acetate copolymer |
| CN101638492A (en) * | 2009-08-31 | 2010-02-03 | 安徽中鼎密封件股份有限公司 | Layered double hydroxide and preparation method of montmorillonite nanometer composite material |
| CN106243735A (en) * | 2016-08-05 | 2016-12-21 | 雷春生 | A kind of preparation method of halogen-free anti-flaming silicon rubber cable sleeve |
| CN109734990A (en) * | 2018-12-28 | 2019-05-10 | 北京理工大学 | Two-dimensional material nano modification flame-proof ethylene-vinyl acetate copolymer method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1752130A (en) * | 2004-09-22 | 2006-03-29 | 北京化工大学 | Fire retardant composite material of nano-aluminium hydroxide, clay and ethylene-vinyl acetate copolymer |
| CN101638492A (en) * | 2009-08-31 | 2010-02-03 | 安徽中鼎密封件股份有限公司 | Layered double hydroxide and preparation method of montmorillonite nanometer composite material |
| CN106243735A (en) * | 2016-08-05 | 2016-12-21 | 雷春生 | A kind of preparation method of halogen-free anti-flaming silicon rubber cable sleeve |
| CN109734990A (en) * | 2018-12-28 | 2019-05-10 | 北京理工大学 | Two-dimensional material nano modification flame-proof ethylene-vinyl acetate copolymer method |
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| CN111808798A (en) * | 2020-09-03 | 2020-10-23 | 朗姿赛尔生物科技（广州）有限公司 | Culture medium for promoting stem cell expansion |
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