CN103073786B - A kind of polypropylene matting agent master batch and its preparation method and application - Google Patents
A kind of polypropylene matting agent master batch and its preparation method and application Download PDFInfo
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- CN103073786B CN103073786B CN201110330624.6A CN201110330624A CN103073786B CN 103073786 B CN103073786 B CN 103073786B CN 201110330624 A CN201110330624 A CN 201110330624A CN 103073786 B CN103073786 B CN 103073786B
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Abstract
The invention provides a kind of polypropylene matting agent master batch and its preparation method and application, relate to modifying plastics field.It includes blended following component: polypropylene, function SBS multipolymer, fully sulfurized silicon rubber powder and silicon-dioxide; Wherein, be 100 parts by weight with polypropylene, function SBS multipolymer 20 ~ 70 weight part; Fully sulfurized silicon rubber powder 10 ~ 50 weight part; Silicon-dioxide 5 ~ 20 weight part; The median size of described fully sulfurized silicon rubber powder is 0.05 ~ 1 μm, and its gel content is 60wt% or higher; The median size of silicon-dioxide is 1 ~ 10 μm.Matting agent master batch prepared in the present invention, significantly can reduce the surface gloss of polypropylene modified material, and in use can require to grasp matting agent master batch consumption flexibly according to the difference of glossiness, using method is simple and reliable, can be widely used in the fields such as superior automobile inside gadget.
Description
Technical field
The present invention relates to a kind of modifying plastics field, say further, relate to a kind of matting agent master batch for reducing polypropylene glossiness and its preparation method and application.
Background technology
It is high that polypropylene has heat resisting temperature, the advantage that fatigue resistance, electrical insulating property, resistance to corrosive chemicals, processing forming are good, and price is low, quality gently, easily reclaims, and is therefore widely used in fields such as automotive industrys.But common modifications polypropylene material has gloss or reflective characteristic more, this defect not only makes automotive trim Integral decoration class reduce, more make car-driver easily tired, even can affect the driving safety of car-driver, increase traffic accident odds, also cannot meet the needs of new automobile Plastics Development that can be decoration integrated.Therefore, automobile low-luster polypropylene material receives publicity day by day.
Around the problem of polypropylene material surface dulling, people have carried out many research work.Publication number CN101759919A patent by adding a kind of mineral filler wollastonite that effectively can reduce product surface glossiness in the basic components of polypropylene composite material, thus prepares low-luster polypropylene composite material.Owing to the addition of a large amount of mineral fillers thus being degrading the comprehensive mechanical property of polypropylene composite material.Publication number CN101173075 patent by adding the glossiness that 0.5 ~ 5 part of silicon-dioxide reduces polypropylene composite material in polypropylene composite material.Equally, addition too much can the mechanical property of deteriorated polypropylene composite material, and addition very little extinction effect is not obvious again, is still difficult to widespread use at present in auto industry field.
Publication number CN101313025A utilized the elastomer copolymer of propylene and ethylene atactic copolymer and propylene and ethene to make comparatively soft polyolefin light extinction composition, this polymkeric substance has good eliminate optical property and mechanical property, be applicable to sheet material extruding, blow thermo forming fields and the field such as internal decoration of car top layer and film, but this composition is not suitable for injection structure product.Publication number CN101121799A patent discloses one and adds peroxide cross-linking agent that polyethylene molecule is produced is crosslinked, forming microgel is distributed in polypropylene matrix, this microgel produces tiny projection at product surface and causes the diffuse-reflectance of light to reduce the glossiness on polypropylene blending modified material surface, but extinction effect is not ideal enough.
Summary of the invention
For problems of the prior art, an object of the present invention is to provide a kind of matting agent master batch for reducing polypropylene glossiness.By adding matting agent master batch provided by the invention, effectively can reduce the surface gloss of modified polypropylene material, solving the deficiencies in the prior art well.
Matting agent master batch of the present invention includes following main ingredient: polypropylene (PP), functionalization styrene-butadiene-styrene block copolymer (function SBS multipolymer), fully sulfurized silicon rubber powder and silicon-dioxide; Wherein, be 100 parts by weight with polypropylene, function SBS multipolymer is 20 ~ 70 weight parts, is preferably 25 ~ 60 weight parts; Fully sulfurized silicon rubber powder is 10 ~ 50 weight parts, is preferably 15 ~ 40 weight parts; Silicon-dioxide is 5 ~ 20 weight parts, is preferably 10 ~ 20 weight parts.
In the present invention, described polypropylene comprises at least one in various homo-polypropylene of the prior art or Co-polypropylene.Its melting index preferably 0.5 ~ 5.0g/10min.
Described function SBS multipolymer is a kind of Tetrablock copolymer, structure can represent with SDSP, wherein S represents polystyrene block, D represents polybutadiene block or polyisoprene blocks, P represents polar block, the polar monomer polymerization that this polar block is made up of the pyridine of vinyl arsenic and derivative thereof obtains, and this polar monomer comprises the pyridine of 2-vinyl arsenic, the arsenic pyridine of 4-vinyl and isomer thereof etc.In the SDS segment of function SBS multipolymer, the ratio of S/D is 5% ~ 95%/95% ~ 5%, and the weight content of polar block is 0.1% ~ 50% in the polymer.The number-average molecular weight of described function SBS is not limit, and is preferably 10,000 ~ 300,000; Molecular weight distributing index is not limit, and is preferably 1.02 ~ 2.00.
Described fully sulfurized silicon rubber powder, its median size is 0.05 ~ 1 μm, preferably 0.05 ~ 0.2 μm, is more preferably 0.05 ~ 0.1 μm; Its gel content is 60wt% or higher, is preferably 75wt% or higher, is more preferably 90wt% or higher.Described fully sulfurized silicon rubber powder particle has the fully sulfurized silicon rubber powder of equal phase structure, and each particulate namely in this fully sulfurized silicon rubber powder is homogeneous phase, and single particulate is all homogeneous on composition.The phenomenon of layering, point equal uneven phase is not found in particulate under the observation of existing microtechnique.This fully sulfurized silicon rubber powder is by fixing silicone rubber latex cross-linking radiation rubber particles particle diameter.Detailed content of fully sulfurized silicon rubber powder of the present invention and preparation method thereof, can see Chinese patent CN 1383439A, and its full content is incorporated herein the present invention as a reference.
Described silicon-dioxide is commercially available silicon-dioxide, and its particle size range is generally unlimited, can be preferably 1 ~ 10 μm.
In the present invention, the fully sulfurized silicon rubber powder added inherently has good rebound resilience and the effect of delustring, therefore plays a role to the glossiness reducing matrix material; And function SBS multipolymer and fully sulfurized silicon rubber powder small especially can be dispersed and form small gel in polypropylene, formed at product surface after shaping and can produce uniform irreflexive minute asperities, thus effectively reduce the glossiness on polypropylene composite material surface.Silicon-dioxide is the inorganics of a kind of small particle size, multiple aperture, bigger serface, is dispersed in polypropylene matrix by mixing facilities, shapingly much stays surface afterwards, forms small male and fomale(M&F), thus reduces the glossiness of material.
Also comprise oxidation inhibitor in matting agent master batch of the present invention, oxidation inhibitor can select various oxidation inhibitor conventional in prior art polypropylene, and its consumption is also conventional amount used.Comparative optimization, described oxidation inhibitor is selected from the mixture of Hinered phenols antioxidant and phosphoric acid ester oxidation inhibitor.Total consumption of oxidation inhibitor is 100 weight parts with polypropylene, is 0.1 ~ 0.5 weight part, preferably 0.2 ~ 0.4 weight part.The weight ratio of described Hinered phenols antioxidant and phosphoric acid ester oxidation inhibitor is 1: 1 ~ 1: 2.Wherein Hinered phenols antioxidant preferably four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (as the anti-oxidant Irganox 1010 that Ciba fine chemicals produces); Phosphoric acid ester oxidation inhibitor is three (2,4-di-tert-butylphenol) phosphorous acid ester (as the Irgafos 168 that Ciba fine chemicals produces) preferably.
Some auxiliary agents conventional in the acrylic resin course of processing can also be comprised in matting agent master batch of the present invention, as: dispersion agent, processing thermo-stabilizer, photostabilizer etc., its consumption is conventional amount used, or adjusts according to the requirement of practical situation.
Two of object of the present invention is to provide above theory to be the preparation method of polypropylene matting agent master batch, is achieved through the following technical solutions: the component comprising described acrylic resin, function SBS, fully sulfurized silicon rubber powder and silicon-dioxide etc. is obtained described polypropylene matting agent master batch by described content melt blending.
Further illustrate the preparation method of this kind of matting agent master batch, comprise the following steps:
The first step: take various described raw material by described consumption;
Second step: by dried acrylic resin, function SBS multipolymer, fully sulfurized silicon rubber powder, silicon-dioxide at interior each component Homogeneous phase mixing in mixing equipment, obtains mixture.
3rd step: namely the mixture that step 2 obtains is made matting agent master batch of the present invention after blending equipment melt blending extruding pelletization.
In the course of processing of matting agent master batch of the present invention, material melts blending temperature is blending temperature used in the processing of usual acrylic resin, should not only ensureing the complete melting of matrix resin but also can not make to select in its scope of decomposing, be generally 190 DEG C ~ 220 DEG C, preferred processing temperature is 200 ~ 220 DEG C.In addition, according to processing needs, in blended material, some auxiliary agents conventional in the acrylic resin course of processing can be added in right amount, as: dispersion agent, processing thermo-stabilizer, photostabilizer etc., its consumption is conventional amount used, or adjusts according to the requirement of practical situation.
In the preparation method of the invention described above, the mixing equipment of mixing of materials can adopt various mixing equipments used in prior art, as stirrer, kneading machine etc.The melt blending equipment used in preparation method of the present invention is the general blending equipment in rubber and plastic processing industry, can be twin screw extruder, the mixing unit of BUSS etc.
Three of object of the present invention is to provide this kind of application of matting agent master batch on low-luster polypropylene is material modified, is achieved through the following technical solutions: by comprise the melt blending extruding pelletizations such as acrylic resin, described matting agent master batch and other conventional constituents the polypropylene modified material of low-luster.Wherein the consumption of matting agent master batch is generally 100 weight parts with acrylic resin, is 10 ~ 40 parts by weight.
Further illustrate the using method of this kind of matting agent master batch, comprise following technological step:
The first step: by described with measuring various raw material;
Second step: be fully mixed to evenly in mixing equipment in interior each component by dried acrylic resin, matting agent master batch and other components, obtains mixture.
3rd step: the polypropylene modified material that namely mixture that step 2 obtains be can be made into after blending equipment melt blending extruding pelletization low-luster.
The processing parameters such as the equipment more than used in application and processing temperature are all with the equipment and process parameter usually adopted in polypropylene manufacture field.
Compared with prior art, the present invention has following beneficial effect:
Use matting agent master batch of the present invention can reduce the surface gloss of polypropylene modified material significantly.And in use can require to grasp matting agent master batch consumption flexibly according to the difference of glossiness, using method is simple and reliable.The fields such as superior automobile inside gadget can be widely used in.
Embodiment
Below in conjunction with specific embodiment, the present invention will be further described.But the present invention is not limited in following embodiment.
Prepared by matting agent master batch:
By matrix resin PP (K8303, Sinopec Yanshan Mountain branch office, melting index 2.5g/10min), (number-average molecular weight is 8.43 ten thousand to function SBS multipolymer, polar block weight content 3.0%, S/D weight ratio is 40/60, molecular weight distributing index is 1.2, and polar monomer is the pyridine of vinyl arsenic; Ba Ling petrochemical complex limited liability company produce), fully sulfurized silicon rubber powder (trade mark VP-602, median size 0.1 μm, gel content 90wt%; Beijing Chemical Research Institute of China Petrochemical Industry produces) and silicon-dioxide (trade mark C807, particle diameter 7 μm, pH value 3.3, porosity 2ml/g; W. R. Grace & Co of the U.S.), oxidation inhibitor (antioxidant 1010 and irgasfos 168 composite, weight ratio 1: 1; Ciba fine chemicals produces) put into homogenizer, stir 3 minutes under the rotating speed of 300 revs/min, each component is fully mixed; Subsequently by the BUSS mixing unit of said mixture material within the scope of 190 DEG C ~ 220 DEG C (MKD-30, BUSS company of Switzerland), extruding pelletization, obtains matting agent master batch.It is specifically filled a prescription in table 1, and wherein each component concentration is all with weight parts.
The component proportion of table 1 matting agent master batch
Prepared by low-luster polypropylene material:
Embodiment 1 ~ 8
By polypropylene (K9020, Sinopec Yanshan Mountain branch office), (Irganox 1010 and Irgafos 168 is composite and obtain with weight ratio 1: 1 for matting agent master batch (A-D) and oxidation inhibitor, Ciba fine chemicals) put into homogenizer, stir 3 minutes under the rotating speed of 300 revs/min, each component is fully mixed.Subsequently by the twin-screw extrusion unit of said mixture material within the scope of 190 DEG C ~ 220 DEG C, extruding pelletization, obtains low-luster polypropylene material modified.It is specifically filled a prescription in table 2, and wherein each component concentration is all with weight parts.
The pellet extruded is dried 6hr in 95 DEG C of constant temperature ovens, then becomes standard batten at the condition hemostasis of 210 DEG C ~ 225 DEG C, carry out the test of eliminate optical property and Izod notched impact strength.The test of Izod notched impact strength is tested according to international standard testing method ISO180.Glossiness test uses JFL-BZ20 ° of 60 ° of 85 ° of intelligent Grossmeters, and test condition is: (1) stability: 0.4 gloss unit (Gs)/30 minute; (2) measurement window size: 16 × 48 (mm); (3) test sample surface is specular light face.Testing standard is ISO-2813.Test result is in table 2.
Embodiment 9 ~ 16
By polypropylene (K9020, Sinopec Yanshan Mountain branch office), matting agent master batch (A-D), superfine talcum powder (median size 6.5 μm, Haicheng powder body material company limited) and oxidation inhibitor (Irganox 1010 and Irgafos 168 is composite and obtain with weight ratio 1: 1, Ciba fine chemicals) put into homogenizer, stir 3 minutes under the rotating speed of 300 revs/min, each component is fully mixed.Subsequently by the twin-screw extrusion unit of said mixture material within the scope of 190 DEG C ~ 220 DEG C, extruding pelletization, obtains low-luster polypropylene material modified.It is specifically filled a prescription in table 3, and wherein each component concentration is all with weight parts.
The pellet extruded is dried 6hr in 95 DEG C of constant temperature ovens, then becomes standard batten at the condition hemostasis of 210 DEG C ~ 225 DEG C, carry out the test of eliminate optical property.Glossiness test uses JFL-BZ 20 ° of 60 ° of 85 ° of intelligent Grossmeters, and test condition is: (1) stability: 0.4 gloss unit (Gs)/30 minute; (2) measurement window size: 16 × 48 (mm); (3) test sample surface is specular light face.Testing standard is ISO-2813.Its test result is in table 3.
Comparative example 1 ~ 3
By polypropylene (with embodiment 1), (comparative example 1 does not add superfine talcum powder, comparative example 2 is with embodiment 9, comparative example 3 is with embodiment 10) and oxidation inhibitor (with embodiment 1) put into homogenizer, stir 3 minutes under the rotating speed of 300 revs/min, each component is fully mixed.Subsequently by the twin-screw extrusion unit of said mixture material within the scope of 190 DEG C ~ 220 DEG C, extruding pelletization, obtains low-luster polypropylene material modified.It is specifically filled a prescription in table 2 and table 3, and wherein each component concentration is all with weight parts.Testing standard is with embodiment 1.
Component and the eliminate optical property of table 2 embodiment 1 ~ 8 and comparative example 1 compare
Component and the eliminate optical property of table 3 embodiment 9 ~ 16 and comparative example 2 ~ 3 compare
As can be seen from table 2 and table 3, with the addition of the low-luster polypropylene that matt master makes material modified, not only there is excellent eliminate optical property, also there is excellent shock strength.The fields such as superior automobile inside gadget can be widely used in.
Claims (12)
1. a polypropylene matting agent master batch, includes blended following component: polypropylene, function SBS multipolymer, fully sulfurized silicon rubber powder and silicon-dioxide; Wherein, be 100 parts by weight with polypropylene, function SBS multipolymer is 25 ~ 60 weight parts; Fully sulfurized silicon rubber powder is 15 ~ 40 weight parts; Silicon-dioxide is 10 ~ 20 weight parts;
Described function SBS multipolymer is a kind of Tetrablock copolymer, structure is SDSP, wherein S is polystyrene block, D is polybutadiene block or polyisoprene blocks, P is polar block, and at least one polymerization in the polar monomer that this polar block is made up of vinyl arsenic pyridine or derivatives thereof obtains;
The median size of described fully sulfurized silicon rubber powder is 0.05 ~ 1 μm; Its gel content is 60wt% or higher.
2. matting agent master batch as claimed in claim 1, is characterized in that:
The median size of described fully sulfurized silicon rubber powder is 0.05 ~ 0.2 μm.
3. matting agent master batch as claimed in claim 1, is characterized in that:
The gel content of described fully sulfurized silicon rubber powder is 75wt% or higher.
4. matting agent master batch as claimed in claim 1, is characterized in that:
Described polypropylene comprises at least one of homo-polypropylene and acrylic resin copolymer, and its melting index is 0.5 ~ 5.0g/10min.
5. matting agent master batch as claimed in claim 1, is characterized in that:
The number-average molecular weight of described SDSP is preferably 1 ~ 300,000; Molecular weight distributing index is preferably 1.02 ~ 2.00.
6. matting agent master batch as claimed in claim 1, is characterized in that:
The polar monomer of the polar block of described formation function SBS multipolymer comprises at least one in the pyridine of 2-vinyl arsenic, the arsenic pyridine of 4-vinyl and isomer thereof.
7. matting agent master batch as claimed in claim 1, is characterized in that:
In the segment of described function SBS multipolymer, the part by weight of S/D is 5% ~ 95%/95% ~ 5%, is 0.1% ~ 50% at the weight content of function SBS multipolymer Semi-polarity block.
8. matting agent master batch as claimed in claim 1, is characterized in that:
The particle size range of described silicon rubber powder is 1 ~ 10 μm.
9. matting agent master batch as claimed in claim 1, is characterized in that:
Including with polypropylene is the oxidation inhibitor of 100 weight parts, 0.1 ~ 0.5 weight part;
Described oxidation inhibitor is selected from Hinered phenols antioxidant and phosphoric acid ester antioxidant mixture, and the weight ratio of Hinered phenols antioxidant and phosphoric acid ester oxidation inhibitor is 1:1 ~ 1:2.
10. matting agent master batch as claimed in claim 9, is characterized in that:
Described Hinered phenols antioxidant is four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester; Described phosphoric acid ester oxidation inhibitor is three (2,4-di-tert-butylphenol) phosphorous acid ester.
The preparation method of 11. 1 kinds of matting agent master batches as described in any one of claim 1 ~ 10, is characterized in that:
The component comprising described polypropylene, function SBS multipolymer, fully sulfurized silicon rubber powder and silicon-dioxide mixed by described content, melt blending obtains described polypropylene matting agent master batch.
12. 1 kinds of matting agent master batch application on low-luster polypropylene is material modified as described in any one of claim 1 ~ 10, comprise the polypropylene modified material component melts blending extrusion granulation containing acrylic resin, described matting agent master batch being obtained described low-luster; Be wherein 100 weight parts with acrylic resin, matting agent master batch is 10 ~ 40 parts by weight.
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| CN104031303B (en) * | 2014-04-02 | 2017-01-11 | 南京淳达科技发展有限公司 | Polyethylene master batch compound additive and preparation method thereof |
| CN106009457A (en) * | 2016-07-28 | 2016-10-12 | 广东天保新材料有限责任公司 | PP matte color masterbatch and application thereof |
| PL243805B1 (en) * | 2018-01-03 | 2023-10-16 | Albert Groenwald | Concentrate of thermoplastic polymer matrix polysiloxane and inorganic filler in the form of the premix or granulated product and method for producing the premix and granulated polysiloxane concentrate |
| CN114181452B (en) * | 2021-10-29 | 2023-10-31 | 金发科技股份有限公司 | Polypropylene composition and preparation method and application thereof |
| CN114891356B (en) * | 2022-06-23 | 2023-06-13 | 盛嘉伦橡塑(河源)有限公司 | Thermoplastic elastomer material and preparation method thereof |
| CN115536929B (en) * | 2022-10-27 | 2023-12-08 | 广东美联新材料股份有限公司 | High-haze HDPE extinction master batch and preparation method thereof |
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| CN101173075A (en) * | 2007-12-04 | 2008-05-07 | 上海金发科技发展有限公司 | Low-luster polypropylene composite material and method for producing the same |
| CN101684189A (en) * | 2008-09-28 | 2010-03-31 | 中国石油化工股份有限公司 | Sprayable and toughened polypropylene composition and preparation method thereof |
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| CN1339531A (en) * | 2000-08-22 | 2002-03-13 | 中国石油化工股份有限公司 | High toughness plastic and its preparing method |
| CN101173075A (en) * | 2007-12-04 | 2008-05-07 | 上海金发科技发展有限公司 | Low-luster polypropylene composite material and method for producing the same |
| CN101684189A (en) * | 2008-09-28 | 2010-03-31 | 中国石油化工股份有限公司 | Sprayable and toughened polypropylene composition and preparation method thereof |
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