CN104629340B - Exempt from spraying PPO resin combinations and its preparation method and application with special decorative effects - Google Patents
Exempt from spraying PPO resin combinations and its preparation method and application with special decorative effects Download PDFInfo
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- CN104629340B CN104629340B CN201310544202.8A CN201310544202A CN104629340B CN 104629340 B CN104629340 B CN 104629340B CN 201310544202 A CN201310544202 A CN 201310544202A CN 104629340 B CN104629340 B CN 104629340B
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Abstract
Exempt to spray PPO resin combinations and its preparation method and application, including following component with special decorative effects the invention discloses a kind of：The 98wt% of PPO resins 70；The 25wt% of polymer overmold special-effect powder microballoon 1；The 10wt% of compatilizer 0；The 1wt% of antioxidant 0.1；The 0.5wt% of processing aid 0.1；The present invention is by redisperse after special-effect powder is overmolding into microballoon with aqueous polymer dispersion into PPO resins, the compatibility of special-effect powder and PPO resins can be obviously improved, eliminate the product current mark that surface is formed in extrusion or injection moulding process and mitigate weld bond, the PPO resin combinations of exempting to spray being prepared have the special aesthetic effects such as obvious metal-like, pearly-lustre flicker, substantially increase the market application for exempting from sprayed on material.
Description
Technical field
The invention belongs to polymeric material field, and in particular to a kind of to exempt from spraying PPO resins with special decorative effects
Composition and its preparation method and application.
Background technology
As people increasingly pay attention to and paid close attention to environmental problem, exempt from spraying special-effect material product and just progressively show
Its competitiveness, gorgeous colorful tone and pearly-lustre, flash effect, metal that spray painting is produced can be replicated by exempting from spraying aesthetic resin
The special-effect such as gloss and texture, so as to meet diversified, differential customer demand, and in process of production can be real
Energy-saving and emission-reduction are realized, can be widely applied to handicraft, toy, household electrical appliances, automobile, electronic product, sports goods and office appliance etc.
Field.
At present, it is that the tool such as metal powder, pearl essence is added in resin material to exempt to spray the more common preparation method of resin
There is the effect powder of particular color and gloss.By the way that special-effect powder is distributed in matrix resin, between special-effect powder mutually
Connection, forms the film of continuous special-effect, has covered base material, show special-effect texture, although by by special-effect
Powder is directly added into resin binder, it is possible to achieve the effect of special gloss, but the compatibility of matrix resin and special-effect powder
Difference, under the conditions of the strong pressure and Strong shear extruded or be molded, special-effect powder is extremely difficult to mobility with base resin material
Unanimously, particularly baroque product, occur along the special-effect powder of flow direction orientation and melt flows steering occur,
Phenomena such as flow velocity is unstable, and melt converges, causes special-effect powder skewness in the melt, easily formed in product surface
The defects of current mark and weld bond, seriously prevent and limit such marketing and application for exempting from sprayed on material.
The content of the invention
The shortcomings that in order to overcome prior art and deficiency, primary and foremost purpose of the invention are that provide one kind melts without current mark, gently
Wiring exempts from spraying PPO resin combinations with special decorative effects.
It is still another object of the present invention to provide the above-mentioned system for exempting to spray PPO resin combinations with special decorative effects
Preparation Method.
The present invention is achieved by the following technical solutions：
Exempt from spraying PPO resin combinations with special decorative effects, by weight percentage, including following component：
PPO resins 70-98wt%
Polymer overmold special-effect powder microballoon 1-25wt%
Compatilizer 0-10wt%
Antioxidant 0.1-1wt%
Processing aid 0.1-0.5wt%；
Wherein, described polymer overmold special-effect powder microballoon, by weight percentage, including following component：
Aqueous polymer dispersion 18-90wt%
Antioxygen corrosion inhibiter 0-5wt%
Special-effect powder, or water-based special-effect slurry material 5-80wt%
Curing agent 0.2-10wt%.
The aqueous polymer dispersion is selected from polystyrene emulsion, acrylic acid ester emulsion, styrene-acrylic emulsion, ABS emulsions, AS
Emulsion, ASA emulsions, MBS emulsions, the one or more of styrene-butadiene emulsion and its modifier.
The solid content of the aqueous polymer dispersion is 10-60wt%.
The compatilizer is selected from ABS grafted maleic anhydrides, the sulfonate of polystyrene, SBS grafted maleic anhydrides, SEBS and connect
The one or more of branch maleic anhydride, SMA or acrylate copolymer；
The antioxidant is to include Hinered phenols antioxidant, phosphite kind antioxidant, amine antioxidants, sulfur-bearing class antioxygen
One or more in agent or metallic salt antioxidant；
The processing aid is silicone series lubricant agent, acid amides series lubricant agent, stearic acid lubricant, TPO lubricant
Or the one or more in ester lubricant.
The antioxygen corrosion inhibiter be selected from phenylpropyl alcohol triazole, phytic acid, phytate, 8-hydroxyquinoline, organic phosphorus compound, phosphoric acid and
One or more of mixing in its derivative or pyrogallic acid.
The special-effect powder includes the one or more in metal powder or pearl essence.
One or more of the metal powder in aluminium powder, copper powder, bronze, silver powder, zinc powder, glass putty, iron powder, nickel powder；
The water-based special-effect slurry material is that water and water-soluble solvent are added in special-effect powder, such as isopropanol, second
Alcohol etc. and other auxiliary agents, its solid content are 10-80wt%, preferably 20-70wt%.
The content of Al elements is no less than 60wt% in the aluminium powder, simultaneously containing Zn, Sn, Ni, Pb, Fe, Mg, Si, Mn, Be,
Cu, Ti or rare earth element one or more；Being shaped as the aluminium powder is spherical, petal, dendriform, snowflake shape, cornflakes
The one or more of shape, silver dollar shape or half silver dollar shape；Its particle diameter is 3-200 μm, preferably 5-100 μm.
It is oxidizable in order to avoid aluminium powder explosive in process, the defects of bad ball milling disperses, used in the present invention
Aluminium powder is to add surface conditioning agent such as lubricant etc. by surface treatment, then ball milling into flake aluminum.
The content of Cu elements is no less than 60wt% in the copper powder, simultaneously containing Zn, Sn, Ni, Be, Al, Mn, Fe, Pb, Si,
P, the one or more of B, Ti or rare earth element；Being shaped as the copper powder is spherical, dendroid or sheet, its particle diameter are 3-200 μ
M, preferably 5-100 μm.
Its cross section of the pearl essence has the physical arrangement similar to pearl, and kernel is the material of low optical refractive index,
Be coated on outer layer is the metal oxide of high index of refraction, and its species specifically includes mica coating pearl essence, bismoclite crystallization
Pearl essence, silica-coating pearl essence, aluminium silicate salt coating pearl essence, boric acid aluminium salt coating pearl essence, bismuth oxide coating pearl
One or more in light powder；The pearl essence surface at least coats layer of metal oxide, and the metal oxide is oxidation
Aluminium, tin ash, titanium dioxide, iron oxide, the one or more of antimony oxide or zinc oxide；The particle diameter of the pearl essence is 5-
500 μm, preferably 5-200 μm.
The present invention, which adds pearl essence, can make the metal-like of frosting more obvious, because pearl essence has spy
Different physical arrangement, when being irradiated by light, pearl effect can be embodied by multipath reflection and interference so that material surface
Reflected light closer to metal-like.
The curing agent is selected from amino resins, aziridine and its derivative, polyisocyanates and its oligomer, poly- carbonization two
The one or more of imines, organosiloxane.
Polymer overmold special-effect powder microballoon of the present invention can also add other auxiliary agents according to being actually needed, such as
Defoamer, dispersant, anti-settling agent etc., its dosage are conventional amount used.
The particle diameter of the polymer overmold special-effect powder microballoon is 10-1000 μm, preferably 10-300 μm；Wherein special effect
The weight percent content that fruit powder accounts for microballoon is 5-80wt%, preferably 5-50wt%.
The preparation method of polymer overmold special-effect powder microballoon of the present invention, specifically includes following steps：
a）First, antioxygen corrosion inhibiter is added under normal temperature in aqueous polymer dispersion, 10-30min is dispersed with stirring, obtains
Dispersion liquid；Under agitation, special-effect powder, or water-based special-effect slurry material are slowly added into dispersion liquid, then
Curing agent is added while stirring, and continues to stir 30-120min, is made special-effect powder fully dispersed and is coated by dispersion liquid, most
The composite dispersion liquid of polymer overmold special-effect powder is made afterwards；
b）By composite dispersion liquid drying process, polymer overmold special-effect powder microballoon is obtained.
Preferably, wherein step（b）Described in drying for spray drying, the intake air temperature of the spray-drying process
For 150-300 DEG C, preferably 170-250 DEG C, air outlet temperature is 50-130 DEG C, preferably 70-100 DEG C.
Preparation method of the present invention that exempt to spray PPO resin combinations with special decorative effects, including it is as follows
Step：Each raw material is inserted into high-speed mixer according to the above ratio to be well mixed；Obtained mixture is inserted into double screw extruder
Middle mixing, pelletizing, packaging, are produced after cooling.
PPO resin combinations of exempting to spray of the present invention with special decorative effects can be in electronic apparatus, physical culture use
It is used widely in product, office appliance, traffic and transport field.
The present invention compared with prior art, has the advantages that：
The present invention passes through redisperse after special-effect powder is overmolding into microballoon with aqueous polymer dispersion to PPO resins
In, the compatibility of special-effect powder and PPO resins can be obviously improved, the endurance of cutting of special-effect powder is improved and its is squeezing
Go out or injection moulding process in flowing uniformity with melt, so as to eliminate the current mark of product surface, mitigate weld bond, be prepared
Exempting from spraying PPO resin combinations has obvious metal-like or special aesthetic effect, substantially increases and exempts from sprayed on material
Market application.
Embodiment
The present invention is further illustrated below by embodiment, following examples are the preferable embodiment party of the present invention
Formula, but embodiments of the present invention are not limited by following embodiments.
The preparation of embodiment 1-6 polymer overmold special-effect powder microballoons：
By the formula in table 1, first, antioxygen corrosion inhibiter is added under normal temperature in aqueous polymer dispersion, is dispersed with stirring
15min, obtain dispersion liquid；Under agitation, special-effect powder, or water-based special-effect powder are slowly added into dispersion liquid
Slurry, curing agent is then added while stirring, and continue to stir 30-120min, make special-effect powder fully dispersed and disperseed
Liquid coats, and the composite dispersion liquid of polymer overmold special-effect powder is finally made；By composite dispersion liquid spray drying treatment, obtain
Polymer overmold special-effect powder microballoon, the intake air temperature of spray-drying process is 150-300 DEG C, air outlet temperature 50-
130℃。
The specific proportioning that the embodiment 1 ~ 6 of table 1 respectively forms（wt%）
In embodiment 1：Aqueous polymer dispersion is polystyrene emulsion, and its solid content is 10wt%；Metal powder is through table
The flake aluminum of face processing, the content of Al elements is 60wt% in aluminium powder, simultaneously containing Zn and Sn；Its particle diameter is 100 μm；Antioxygen
Corrosion inhibiter is pyrogallic acid；Curing agent is aziridine.
In embodiment 2：Aqueous polymer dispersion is styrene-acrylic emulsion, and its solid content is 60wt%；Metal powder be through surface at
The flake copper of reason, the content of Cu elements is 70wt% in copper powder, simultaneously containing Zn and Sn；Its particle diameter is 5 μm；Antioxygen corrosion inhibiter
For phenylpropyl alcohol triazole；Curing agent is amino resins.
In embodiment 3：Aqueous polymer dispersion is ABS emulsions, and its solid content is 40wt%；Special-effect powder is dioxy
SiClx coats pearl essence, and its particle diameter is 20 μm；Curing agent is polyisocyanates.
In embodiment 4：Aqueous polymer dispersion is AS emulsions, and its solid content is 50wt%；Special-effect powder applies for mica
Pearl essence is covered, its particle diameter is 200 μm；Curing agent is aziridine.
In embodiment 5：Aqueous polymer dispersion is ASA emulsions, and its solid content is 30wt%；Special-effect powder is zinc powder
With the mixture of silica-coating pearl essence；Curing agent is polycarbodiimide.
In embodiment 6：Aqueous polymer dispersion is MBS emulsions, and its solid content is 20wt%；Special-effect powder is silver powder
With the mixture of mica coating pearl essence；Curing agent is organosiloxane.
Embodiment 7-13 has the preparation for exempting to spray PPO resin combinations of special decorative effects：
By the formula in table 2 by PPO resins, polymer overmold special-effect powder microballoon, compatilizer, antioxidant, processing
Auxiliary agent is inserted high-speed mixer and is well mixed；Obtained mixture is inserted in double screw extruder and is kneaded, pelletizing, bag after cooling
Dress, is produced.Acquired results are shown in Table 2：
Compatilizer is SEBS grafted maleic anhydrides；
Antioxidant is hindered phenol antioxygen 1010 and phosphoric acid ester irgasfos 168；
Processing aid is pentaerythrite stearic acid.
Comparative example 1-6：Tradition is exempted to spray the preparation of PPO resin combinations：
PPO resins resinoid, special-effect powder, compatilizer, antioxidant, processing aid are inserted by the formula in table 2
High-speed mixer is well mixed；Obtained mixture is inserted in double screw extruder and is kneaded, pelletizing, packaging, are produced after cooling.
Acquired results are shown in Table 2：
In comparative example 1：Metal powder is surface treated flake aluminum, and the content of Al elements is 60wt% in aluminium powder, simultaneously
Contain Zn and Sn；Its particle diameter is 100 μm；
In comparative example 2：Metal powder is surface treated flake aluminum, and the content of Al elements is 60wt% in aluminium powder, simultaneously
Contain Zn and Sn；Its particle diameter is 100 μm；
In comparative example 3：Metal powder is surface treated flake copper, and the content of Cu elements is 70wt% in copper powder, simultaneously
Contain Zn and Sn；Its particle diameter is 5 μm；
In comparative example 4：Special-effect powder is silica-coating pearl essence, and its particle diameter is 20 μm；
In comparative example 5：Special-effect powder is that mica coats pearl essence；
In comparative example 6：Special-effect powder is the mixture of zinc powder and silica-coating pearl essence.
The specific proportioning respectively formed in the embodiment 7-13 of table 2 and comparative example 1-6（wt%）And its test performance result
Note：+ more expression current marks are more
More than zero represents that weld bond is more serious
- represent that current mark or weld bond, or unobvious are not present
It can be seen from the Comparative result in upper table 2 in the case where ensureing that other components and content are essentially identical, implement
Example 7-12 is mixed using polymer overmold special-effect powder microballoon with matrix resin, in comparative example 1-6 that special-effect powder is direct
It is added in matrix resin, comparing embodiment 7-11 and comparative example 1-5, finds micro- with polymer-coated metal powder and pearl essence
Ball mixes the product surface of gained with matrix resin substantially without current mark, and weld bond is lighter, and has more preferable aesthetic effect.
Claims (19)
1. exempt from spraying PPO resin combinations with special decorative effects, by weight percentage, including following component：
PPO resins 70-98wt%
Polymer overmold special-effect powder microballoon 1-25wt%
Compatilizer 0-10wt%
Antioxidant 0.1-1wt%
Processing aid 0.1-0.5wt%；
Wherein, described polymer overmold special-effect powder microballoon, by weight percentage, including following component：
Aqueous polymer dispersion 18-90wt%
Antioxygen corrosion inhibiter 0-5wt%
Special-effect powder, or water-based special-effect slurry material 5-80wt%
Curing agent 0.2-10wt%
The content of the antioxygen corrosion inhibiter is not 0, selected from phenylpropyl alcohol triazole, phytic acid, phytate, 8-hydroxyquinoline, organic phosphine
One or more of mixing in thing, phosphoric acid and its derivative, pyrogallic acid；
The special-effect powder includes the one or more in metal powder or pearl essence；
The water-based special-effect slurry material is that water and water-soluble solvent and other auxiliary agents are added in special-effect powder.
2. according to claim 1 exempt from spraying PPO resin combinations with special decorative effects, it is characterised in that institute
State aqueous polymer dispersion and be selected from polystyrene emulsion, acrylic acid ester emulsion, styrene-acrylic emulsion, ABS emulsions, AS emulsions, ASA breasts
Liquid, MBS emulsions, the one or more of styrene-butadiene emulsion and its modifier；The solid content of the aqueous polymer dispersion is 10-
60wt%。
3. according to claim 1 exempt from spraying PPO resin combinations with special decorative effects, it is characterised in that institute
State compatilizer and be selected from ABS grafted maleic anhydrides, the sulfonate of polystyrene, SBS grafted maleic anhydrides, SEBS grafted maleics
The one or more of acid anhydride, SMA or acrylate copolymer；The antioxidant is to include Hinered phenols antioxidant, phosphite
Kind antioxidant, amine antioxidants, containing the one or more in sulfur type antioxidant or metallic salt antioxidant；The processing aid is
Silicone series lubricant agent, acid amides series lubricant agent, stearic acid lubricant, TPO lubricant or one kind in ester lubricant or
It is several.
4. according to claim 1 exempt from spraying PPO resin combinations with special decorative effects, it is characterised in that institute
State one or more of the metal powder in aluminium powder, copper powder, bronze, silver powder, zinc powder, glass putty, iron powder, nickel powder；The water-based spy
The solid content of special effect fruit powder slurry is 10-80wt%.
5. according to claim 4 exempt from spraying PPO resin combinations with special decorative effects, it is characterised in that institute
The solid content for stating water-based special-effect slurry material is 20-70wt%.
6. according to claim 4 exempt from spraying PPO resin combinations with special decorative effects, it is characterised in that institute
The content for stating Al elements in aluminium powder is no less than 60wt%, simultaneously containing Zn, Sn, Ni, Pb, Fe, Mg, Si, Mn, Be, Cu, Ti or dilute
The one or more of earth elements；Being shaped as the aluminium powder is spherical, petal, dendriform, snowflake shape, cornflakes shape, silver dollar shape
Or half silver dollar shape one or more；Its particle diameter is 3-200 μm.
7. according to claim 6 exempt from spraying PPO resin combinations with special decorative effects, it is characterised in that institute
The particle diameter for stating aluminium powder is 5-100 μm.
8. according to claim 4 exempt from spraying PPO resin combinations with special decorative effects, it is characterised in that institute
The content for stating Cu elements in copper powder is no less than 60wt%, simultaneously containing Zn, Sn, Ni, Be, Al, Mn, Fe, Pb, Si, P, B, Ti or dilute
The one or more of earth elements；Being shaped as the copper powder is spherical, dendroid or sheet, its particle diameter are 3-200 μm.
9. according to claim 8 exempt from spraying PPO resin combinations with special decorative effects, it is characterised in that institute
The particle diameter for stating copper powder is 5-100 μm.
10. according to claim 1 exempt from spraying PPO resin combinations with special decorative effects, it is characterised in that institute
Stating pearl essence includes mica coating pearl essence, bismoclite crystallization pearl essence, silica-coating pearl essence, aluminium silicate salt coating
One or more in pearl essence, boric acid aluminium salt coating pearl essence, bismuth oxide coating pearl essence；At least wrap on the pearl essence surface
Layer of metal oxide is covered, the metal oxide is aluminum oxide, tin ash, titanium dioxide, iron oxide, antimony oxide or oxidation
The one or more of zinc；The particle diameter of the pearl essence is 5-500 μm.
11. according to claim 10 exempt from spraying PPO resin combinations with special decorative effects, it is characterised in that
5-200 μm of the particle diameter of the pearl essence.
12. according to claim 1 exempt from spraying PPO resin combinations with special decorative effects, it is characterised in that institute
State curing agent and be selected from hexamethylenetetramine, ammonium chloride, polyisocyanates and its oligomer, amino resins, organosiloxane, nitrogen third
Pyridine and its derivative, the one or more of polycarbodiimide.
13. according to claim 1 exempt from spraying PPO resin combinations with special decorative effects, it is characterised in that institute
The particle diameter for stating polymer overmold special-effect powder microballoon is 10-1000 μm；Wherein special-effect powder accounts for the percentage by weight of microballoon
Content is 5-80wt%.
14. according to claim 13 exempt from spraying PPO resin combinations with special decorative effects, it is characterised in that
The particle diameter of the polymer overmold special-effect powder microballoon is 10-300 μm；Wherein special-effect powder accounts for the percentage by weight of microballoon
Content is 5-50wt%.
15. according to claim 1 exempt from spraying PPO resin combinations with special decorative effects, it is characterised in that institute
The preparation method of polymer overmold special-effect powder microballoon is stated, specifically includes following steps：
a）First, antioxygen corrosion inhibiter is added under normal temperature in aqueous polymer dispersion, 10-30min is dispersed with stirring, is disperseed
Liquid；Under agitation, special-effect powder, or water-based special-effect slurry material are slowly added into dispersion liquid, then side is stirred
Mix side and add curing agent, and continue to stir 30-120min, make special-effect powder fully dispersed and coated by dispersion liquid, finally made
Obtain the composite dispersion liquid of polymer overmold special-effect powder；
b）By composite dispersion liquid drying process, polymer overmold special-effect powder microballoon is obtained.
16. exempt from spraying PPO resin combinations with special decorative effects described in claim 15, it is characterised in that step
（b）Described in drying be spray drying, the intake air temperature of the spray-drying process is 150-300 DEG C, air outlet temperature
For 50-130 DEG C.
17. exempt from spraying PPO resin combinations with special decorative effects described in claim 16, it is characterised in that described
The intake air temperature of spray-drying process is 170-250 DEG C, and air outlet temperature is 70-100 DEG C.
18. the preparation side for exempting to spray PPO resin combinations with special decorative effects described in claim any one of 1-17
Method, it is characterised in that comprise the following steps：Each raw material is inserted into high-speed mixer in the ratio to be well mixed；By what is obtained
Mixture is inserted in double screw extruder and is kneaded, and pelletizing, packaging, are produced after cooling.
19. exempt to spray PPO resin combinations in electronics electricity with special decorative effects described in claim any one of 1-17
Application in device, sports goods, office appliance, traffic and transport field.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102516700A (en) * | 2011-12-09 | 2012-06-27 | 上海锦湖日丽塑料有限公司 | Appearance-improving spraying-free aesthetic resin and its preparation method |
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| US7312257B2 (en) * | 2003-01-23 | 2007-12-25 | General Electric Company | Polymer encapsulation of high aspect ratio materials and methods of making same |
| CN102051611B (en) * | 2010-12-31 | 2012-07-11 | 大连工业大学 | Metal surface treating agent |
| CN102585366B (en) * | 2012-02-16 | 2014-06-11 | 金发科技股份有限公司 | Polypropylene composition with copper-colored metal texture, and preparation method and application thereof |
| CN102643505B (en) * | 2012-03-19 | 2014-06-18 | 上海锦湖日丽塑料有限公司 | Spraying-free aesthetic resin composition with magnetism and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102516700A (en) * | 2011-12-09 | 2012-06-27 | 上海锦湖日丽塑料有限公司 | Appearance-improving spraying-free aesthetic resin and its preparation method |
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