CN107200868B - A kind of mica compounded mix, preparation method and applications - Google Patents
A kind of mica compounded mix, preparation method and applications Download PDFInfo
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- CN107200868B CN107200868B CN201710474356.2A CN201710474356A CN107200868B CN 107200868 B CN107200868 B CN 107200868B CN 201710474356 A CN201710474356 A CN 201710474356A CN 107200868 B CN107200868 B CN 107200868B
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
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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
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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Abstract
The present invention relates to a kind of mica compounded mix, preparation method and applications, mica compounded mix is by mica powder and is coated on the nano-TiO on mica powder surface2Composition；After cladding, nano-TiO2Outer surface be rough surface.The technical program is by using nano-TiO on the surface of mica powder2After cladding, the problem of originally its sharp keen corner angle of mica powder surface become to be passivated, and smooth mica powder crystal outer surface also becomes coarse, alleviates stress raisers in composite material resulting from.It is coated on the nano-TiO on mica powder surface simultaneously2The interface interaction power between filler and polyolefin substrate is also enhanced, to promote the mechanical property of composite polyolefine material.
Description
Technical field
The invention belongs to field of material technology, a kind of novel mica compounded mix, preparation method and applications are particularly related to.
Background technique
All the time, mica powder has a wide range of applications in high molecular material, and mica powder enhances polymer for toughening
It is the technical solution that recent studies in recent years developed.
But mica powder is when being added in polymer because there are sharp corner angle on the surface of mica powder, and its with
Polymer, because of amalgamation problem between the two, causes the material internal for the polymer that mica powder is added to be deposited in mixed process
In stress raisers problem, and the raising of the mechanical property of polymer is caused to be restricted.
Summary of the invention
The object of the present invention is to provide a kind of mica compounded mix, preparation method and its applications, to solve composite material
The problems in stress collection is being locally present in inside.
The present invention is achieved by the following technical solutions:
A kind of mica compounded mix by mica powder and is coated on the nano-TiO on the mica powder surface2Composition；
After cladding, the nano-TiO2Outer surface be rough surface.
The mica powder is muscovite, and the partial size of the mica powder is 6-10 μm.
The preparation method of above-mentioned mica compounded mix, comprising the following steps:
1) mica powder is dry, sufficiently remove the moisture of the mica powder adsorption；
2) by meta-titanium perborate, it is dry after the mica powder and polyethylene glycol be added in ethanol water, make the cloud
Female powder is completely dissolved；
3) it is slowly added dropwise saturated ammonium chloride solution under stirring, stands after setting time by centrifugation, filtering, does
Dry, crushing, obtains mica compounded mix.
It is the dry 3-5h in 90-110 DEG C of baking oven to the drying of the mica powder in step 1).
The meta-titanium perborate, the mica powder, the polyethylene glycol and the saturated ammonium chloride solution mass ratio be
(40-60): (120-180): (4-8): (20-30).
In step 2), by meta-titanium perborate, it is dry after the mica powder and polyethylene glycol be added in ethanol water, in
It is made it completely dissolved after 10-12h in the thermostat water bath that temperature is 80-100 DEG C.
The standing setting time is 2h.
A kind of application of mica compounded mix, mica compounded mix described in any of the above-described are used for improved polyalkene.
The beneficial effects of the present invention are:
The technical program is by using nano-TiO on the surface of mica powder2After cladding, originally its is sharp keen on mica powder surface
Corner angle become to be passivated, and smooth mica powder crystal outer surface also becomes coarse, alleviate part in composite material resulting from
The problems in stress collection.It is coated on the nano-TiO on mica powder surface simultaneously2Also enhance the boundary between filler and polyolefin substrate
Face active force, to promote the mechanical property of composite polyolefine material.
Specific embodiment
Carry out the technical solution that the present invention will be described in detail by the following examples, embodiment below is merely exemplary, only
It can be used to explanation and illustration technical solution of the present invention, and be not to be construed as the limitation to technical solution of the present invention.
Raw material used in embodiments herein is as follows:
PBT (model 2002U), Polyplastics；PP (model Z30S), Maoming Petrochemical；PE (model 5070), Panjin ethylene；
PA6 (model C M1017), toray；PS (model 350), Taiwan state are tall；Meta-titanium perborate, Hubei Bang Sheng Chemical Co., Ltd.；
Mica powder, Shijiazhuang Ma Yue mica powder factory；Polyethylene glycol, Hai'an petrochemical industry；Ammonium chloride, the limited public affairs of the environmentally friendly industry in Zhuzhou river sea
Department.
Test equipment use herein is as follows:
ZSK30 type double screw extruder, German W&P company；JL-1000 type tensile testing machine, the wide just experiment instrument in Guangzhou
The production of device company；HTL900-T-5B type injection (mo(u)lding) machine, the production of Hai Tai plastics machinery Co., Ltd；XCJ-500 type shock-testing
Machine, the production of Chengde testing machine factory；QT-1196 type tester for elongation, Dongguan City Gao Tai detecting instrument Co., Ltd；QD-GJS-
B12K type high-speed mixer, Beijing perseverance Order instrument and meter Co., Ltd.
A kind of mica compounded mix by mica powder and is coated on the nano-TiO on mica powder surface2Composition；
After cladding, nano-TiO2Outer surface be rough surface.
Mica powder is muscovite, and the partial size of mica powder is 6-10 μm.
The preparation method of above-mentioned mica compounded mix, comprising the following steps:
1) by mica powder in 90-110 DEG C of baking oven dry 3-5h, sufficiently remove the absorption water on mica powder surface in case
With；
2) by meta-titanium perborate, it is dry after mica powder and polyethylene glycol be added in ethanol water, in temperature be 80-
Mica powder is completely dissolved after 10-12h in 100 DEG C of thermostat water bath；
3) be slowly added dropwise saturated ammonium chloride solution under electric mixer stirring, stand after 2h by centrifugation, filtering,
Dry, crushing, obtains mica compounded mix.
Meta-titanium perborate, mica powder, polyethylene glycol and saturated ammonium chloride solution mass ratio be (40-60): (120-180):
(4-8): (20-30).
A kind of application of mica compounded mix, any of the above-described mica compounded mix are used for improved polyalkene.
Embodiment 1
1) muscovite that partial size is 6 μm is dried into 90 DEG C of baking oven 3h, sufficiently removes the absorption water on mica powder surface
With spare.
2) 400g meta-titanium perborate, 1.2kg mica powder and 40g polyethylene glycol are put into ethanol water, in temperature be 80
DEG C thermostat water bath in be completely dissolved mica powder after 10h.
3) 200g saturated ammonium chloride solution is slowly added dropwise under electric mixer stirring, is centrifuged, filtering, does after standing 2h
Dry, crushing, obtains mica compounded mix P1.
Application examples 1
It takes 20 parts of P1 to be added in 80 parts of polypropylene (PP), stirs 10min through high mixer, be subsequently added into double screw extruder
Middle carry out blending extrusion, obtains PP composite material 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 220 DEG C, and the temperature of third humidity province is 230 DEG C, and the temperature of the 4th humidity province is 240 DEG C, the 5th temperature
The temperature for spending 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 230 DEG C, screw rod
Revolving speed is 220r/min.
Comparative example 1
It takes 20 parts of muscovites to be added in 80 parts of polypropylene (PP), stirs 10min through high mixer, be subsequently added into twin-screw and squeeze
Blending extrusion is carried out in machine out, obtains mica powder/PP composite material D1.
Batten, properties of product data are made with injection molding machine in PP composite material prepared by above application examples 1 and comparative example 1
It is as shown in the table:
As can be seen from the above table:
The tensile strength of X1, bending strength, cantilever beam impact strength ratio D1 it is big, this illustrates that P1 MODIFIED PP ratio is added
The simple physical property that mica powder is added is more preferable.
Embodiment 2
1) muscovite dry 5h, the abundant absorption for removing mica powder surface in 110 DEG C of baking oven for being 10 μm by partial size
Water is with spare.
2) 600g meta-titanium perborate, 1.8kg mica powder and 80g polyethylene glycol are put into ethanol water, in temperature be 100
DEG C thermostat water bath in be completely dissolved mica powder after 12h.
(3) 300g saturated ammonium chloride solution is slowly added dropwise under electric mixer stirring, is centrifuged, filtering, does after standing 2h
Dry, crushing, obtains mica compounded mix P2.
Application examples 2
It takes 20 parts of P2 to be added in 80 parts of polybutylene terephthalate (PBT)s (PBT), stirs 10min through high mixer, then
Carry out blending extrusion is added twin-screw extrude, PBT composite X2 is obtained.
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 260 DEG C, and the temperature of third humidity province is 260 DEG C, and the temperature of the 4th humidity province is 260 DEG C, the 5th temperature
The temperature for spending area is 260 DEG C, and the temperature of the 6th humidity province is 260 DEG C, and the head temperature of double screw extruder is 260 DEG C, screw rod
Revolving speed is 300r/min.
Comparative example 2
It takes 20 parts of muscovites to be added in 80 parts of PBT, stirs 10min through high mixer, be subsequently added into double screw extruder
Blending extrusion is carried out, mica/PBT composite D2 is obtained.
Batten, properties of product number is made with injection molding machine in PBT composite prepared by above application examples 2 and comparative example 2
According to as shown in the table:
As can be seen from the above table:
The tensile strength of X2, bending strength, cantilever beam impact strength ratio D2 it is big, this illustrates that P2 modified PBT is added
Physical property than mica is added merely is more preferable.
Embodiment 3
1) muscovite that partial size is 8 μm is dried into 100 DEG C of baking oven 4h, sufficiently removes the absorption water on mica powder surface
With spare.
2) 500g meta-titanium perborate, 1.5kg mica powder and 60g polyethylene glycol are put into ethanol water, in temperature be 90
DEG C thermostat water bath in be completely dissolved mica powder after 11h.
3) 250g saturated ammonium chloride solution is slowly added dropwise under electric mixer stirring, is centrifuged, filtering, does after standing 2h
Dry, crushing, obtains mica compounded mix P3.
Application examples 3
It takes 20 parts of P3 to be added in 80 parts of polyethylene (PE), stirs 10min through high mixer, be subsequently added into double screw extruder
Middle carry out blending extrusion, obtains PE composite material 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 180 DEG C, and the temperature of third humidity province is 180 DEG C, and the temperature of the 4th humidity province is 180 DEG C, the 5th temperature
The temperature for spending area is 180 DEG C, and the temperature of the 6th humidity province is 180 DEG C, and the head temperature of double screw extruder is 180 DEG C, screw rod
Revolving speed is 300r/min.
Comparative example 3
Take 20 parts of muscovites to be added in 80 parts of PE, stir 10min through high mixer, be subsequently added into double screw extruder into
Row blending extrusion obtains mica/PE composite material D3.
Batten, properties of product data are made with injection molding machine in PE composite material prepared by above application examples 3 and comparative example 3
It is as shown in the table:
As can be seen from the above table:
The tensile strength of X3, bending strength, cantilever beam impact strength ratio D3 it is big, this illustrates that P3 modified PE ratio is added
The simple physical property that mica is added is more preferable.
Embodiment 4
1) muscovite that partial size is 7 μm is dried into 95 DEG C of baking oven 3h, sufficiently removes the absorption water on mica powder surface
With spare.
2) 450g meta-titanium perborate, 1.4kg mica powder and 50g polyethylene glycol are put into ethanol water, in temperature be 80
DEG C thermostat water bath in be completely dissolved mica powder after 12h.
3) 230g saturated ammonium chloride solution is slowly added dropwise under electric mixer stirring, is centrifuged, filtering, does after standing 2h
Dry, crushing, obtains mica compounded mix P4.
Application examples 4
It takes 20 parts of P4 to be added in 80 parts of polyamide 6s (PA6), stirs 10min through high mixer, be subsequently added into twin-screw extrusion
Blending extrusion is carried out in machine, obtains PA6 composite material X4.
Wherein, double screw extruder includes six humidity provinces sequentially arranged, and the temperature of the first humidity province is 130 DEG C, the
The temperature of two humidity provinces is 260 DEG C, and the temperature of third humidity province is 260 DEG C, and the temperature of the 4th humidity province is 260 DEG C, the 5th temperature
The temperature for spending area is 260 DEG C, and the temperature of the 6th humidity province is 260 DEG C, and the head temperature of double screw extruder is 250 DEG C, screw rod
Revolving speed is 320r/min.
Comparative example 4
It takes 20 parts of muscovites to be added in 80 parts of PA6, stirs 10min through high mixer, be subsequently added into double screw extruder
Blending extrusion is carried out, mica/PA6 composite material D4 is obtained.
Batten, properties of product number is made with injection molding machine in PA6 composite material prepared by above application examples 4 and comparative example 4
According to as shown in the table:
As can be seen from the above table:
The tensile strength of X4, bending strength, cantilever beam impact strength ratio D4 it is big, this illustrates that P4 modified Pa 6 is added
Physical property than mica is added merely is more preferable.
Embodiment 5
1) muscovite that partial size is 9 μm is dried into 105 DEG C of baking oven 3h, sufficiently removes the absorption water on mica powder surface
With spare.
2) 560g meta-titanium perborate, 1.6kg mica powder and 70g polyethylene glycol are put into ethanol water, in temperature be 95
DEG C thermostat water bath in be completely dissolved mica powder after 11h.
3) 280g saturated ammonium chloride solution is slowly added dropwise under electric mixer stirring, is centrifuged, filtering, does after standing 2h
Dry, crushing, obtains mica compounded mix P5.
Application examples 5
It takes 20 parts of P5 to be added in 80 parts of styrene (PS), stirs 10min through high mixer, be subsequently added into double screw extruder
Middle carry out blending extrusion, obtains PS composite material 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 third humidity province is 200 DEG C, and the temperature of the 4th humidity province is 200 DEG C, the 5th temperature
The temperature for spending 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
Revolving speed is 280r/min.
Comparative example 5
Take 20 parts of muscovites to be added in 80 parts of PS, stir 10min through high mixer, be subsequently added into double screw extruder into
Row blending extrusion obtains mica/PS composite material D5.
Batten, properties of product data are made with injection molding machine in PS composite material prepared by above application examples 5 and comparative example 5
It is as shown in the table:
As can be seen from the above table:
The tensile strength of X5, bending strength, cantilever beam impact strength ratio D5 it is big, this illustrates that the modified PS ratio of P5 is added
The simple physical property that mica is added is more preferable.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And deformation, the scope of the present invention are extremely equally limited by appended claims.
Claims (5)
1. a kind of preparation method of mica compounded mix, it is characterised in that: the following steps are included:
1) mica powder is dry, sufficiently remove the moisture of the mica powder adsorption；
2) by meta-titanium perborate, it is dry after the mica powder and polyethylene glycol be added in ethanol water, make the mica powder
It is completely dissolved；
3) it is slowly added dropwise saturated ammonium chloride solution under stirring, stands after setting time by centrifugation, filtering, drying, powder
It is broken, obtain mica compounded mix.
2. the preparation method of mica compounded mix according to claim 1, it is characterised in that: to the cloud in step 1)
The drying of female powder is the dry 3-5h in 90-110 DEG C of baking oven.
3. the preparation method of mica compounded mix according to claim 1, it is characterised in that: the meta-titanium perborate, described
The mass ratio of mica powder, the polyethylene glycol and the saturated ammonium chloride solution is (40-60): (120-180): (4-8): (20-
30)。
4. the preparation method of mica compounded mix according to claim 1, it is characterised in that: in step 2), by metatitanic acid
The mica powder and polyethylene glycol after sodium, drying are added in ethanol water, the water bath with thermostatic control for being 80-100 DEG C in temperature
It is made it completely dissolved after 10-12h in pot.
5. the preparation method of mica compounded mix according to claim 1, it is characterised in that: the standing setting time is
2h。
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| CN108329525A (en) * | 2018-03-21 | 2018-07-27 | 安徽江淮汽车集团股份有限公司 | A kind of preparation method of novel Wollastonite Composite Fillers |
| CN108795031B (en) * | 2018-08-28 | 2020-12-01 | 安徽江淮汽车集团股份有限公司 | High-performance PA6 composite material and preparation method thereof |
| CN110982174A (en) * | 2019-11-29 | 2020-04-10 | 苏州润佳高分子材料有限公司 | Shallow sink mark reinforced polypropylene material for automobile |
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|---|---|---|---|---|
| CN101565201A (en) * | 2009-05-05 | 2009-10-28 | 江西添光化工有限责任公司 | Preparation of white titanium pigment double action crystal seed from metatitanic acid |
| CN102491647A (en) * | 2011-11-24 | 2012-06-13 | 盐城工学院 | Preparation method for high emissivity thermal insulation filler with core-shell structure |
| CN105542517A (en) * | 2016-01-14 | 2016-05-04 | 广西七色珠光材料股份有限公司 | White and interference-color matte flaky cored pigment and preparation method thereof |
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2017
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101565201A (en) * | 2009-05-05 | 2009-10-28 | 江西添光化工有限责任公司 | Preparation of white titanium pigment double action crystal seed from metatitanic acid |
| CN102491647A (en) * | 2011-11-24 | 2012-06-13 | 盐城工学院 | Preparation method for high emissivity thermal insulation filler with core-shell structure |
| CN105542517A (en) * | 2016-01-14 | 2016-05-04 | 广西七色珠光材料股份有限公司 | White and interference-color matte flaky cored pigment and preparation method thereof |
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