CN102952329A - Polypropylene composition and preparation method thereof - Google Patents
Polypropylene composition and preparation method thereof Download PDFInfo
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- CN102952329A CN102952329A CN2011102521230A CN201110252123A CN102952329A CN 102952329 A CN102952329 A CN 102952329A CN 2011102521230 A CN2011102521230 A CN 2011102521230A CN 201110252123 A CN201110252123 A CN 201110252123A CN 102952329 A CN102952329 A CN 102952329A
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Abstract
The invention belongs to the field of polypropylene modification, and particularly relates to a polypropylene composition and a preparation method thereof. The polypropylene composition provided by the invention is prepared from the following raw materials in parts by weight: 100 parts of polypropylene resin, 0.05-2% of heat stabilizer, 0.02-0.5 part of stearic acid metal salt, 0.05-3 parts of inorganic filler and 0.01-0.2 part of organic nucleating agent. The polypropylene resin composition, which is prepared by blending and granulating the polypropylene resin, heat stabilizer, stearic acid metal salt, inorganic filler and slight nucleating agent, has the advantages of high rigidity, high heat resistance and low cost; the preparation technique is simple and easy to implement; and the polypropylene resin composition can be used in the fields of automobiles, home appliances, home furnishing and the like.
Description
Technical field
The invention belongs to the polypropylene modification field, be specifically related to a kind of polypropene composition and preparation method thereof.
Background technology
Acrylic resin is owing to having good rigidity and resistance toheat, and the post-modification means are abundant, therefore just progressively substitutes some engineering plastics, is widely used in the fields such as automobile, household electrical appliances and household.Especially the crushing-resistant copolymerization acrylic resin owing to the progress of production technique and catalyst technology, has given product more excellent over-all properties.But because the polyacrylic production of crushing-resistant copolymerization has larger technical difficulty, especially at aspects such as product rigidity, toughness and flowabilities, can't satisfy the demand in some field fully, therefore also need to carry out post-modification on the basis of the existing trade mark of crushing-resistant copolymerization polypropylene, namely realize high rigidity, high tenacity and the high workability etc. of material by adding nucleator, elastomerics, mineral filler, degradation agents etc.
The raising of polypropylene material rigidity obtains by the mode that adds nucleator or mineral filler usually.
Increase along with add-ons such as mineral filler such as calcium carbonate, talcum powder, mica, diatomite, flexural strength and the bending elastic modulus of acrylic resin progressively improve, but can reduce polyacrylic elongation and shock strength simultaneously, affect the color and luster of polypropylene articles and shrinking percentage etc., and the density that adds affiliation raising material of high amount of inorganic filler, restricted the lightweight of goods, especially be restricted in automobile-used field.
In recent years, the application of nucleator in polypropylene progressively strengthens, a lot of petrochemical plant add nucleator in the granulation process of producing acrylic resin, not only the adding of nucleator polyacrylic color and luster is had no adverse effects, and can improve thermotolerance and the glossiness of acrylic resin.Usually add-on is 0.05%～0.5%, although addition is little, because nucleator expensive (according to quality product and state of the art, price does not wait tens0000 to 500,000 usually) can increase acrylic resin ton cost hundreds of unit.
Document (synthetic and rigidity enhanced, modified polypropylene petrochemical technology and the application of metal carboxylate nucleator, 2007, Vol.25, No.4) add crystal property, thermal characteristics and bending elastic modulus that 0.3～0.5% metal carboxylate nucleator improves material in the pure homo-polypropylene resin.
Document (nucleator on the impact of high-gloss polypropylene performance, plastics industry, 2009, Vol37, supplementary issue S1) adds the bending elastic modulus that 0.2% dissimilar nucleator improves material in homo-polypropylene.
Document (impact of nanometer phosphoric acid ester Nucleating Agent On The Polypropylene Property, modern plastics processed and applied, 2008, Vol.20, No.4) adds nanometer phosphoric acid ester nucleator 0.1%～0.2%, improves the block copolymerization polypropylene bending elastic modulus.
Patents CN101190988A discloses a kind of high gloss heat-resistance polypropylene resin combination, contains homo-polypropylene in the prescription, 0.04～0.1% nucleator, and 0.04～0.08% lubricant, 0.06～0.12% oxidation inhibitor etc. do not contain mineral filler.
Prior art improves the rigidity of acrylic resin and resistance toheat etc. by adding a large amount of nucleators, and cost is higher.
Summary of the invention
Technical problem to be solved by this invention provides a kind of polypropylene resin composite and preparation method thereof, this polypropylene resin composite is by adopting when the granulation composite mode to add a small amount of nucleator and a small amount of mineral filler, and the polypropylene resin composite of making has high rigidity, height is heat-resisting and cost is low advantage.
Polypropene composition of the present invention, made by the raw material of following parts by weight:
Acrylic resin: 100
Thermo-stabilizer: 0.05～2
Metallic stearates: 0.02～0.5
Mineral filler: 0.05～3
Organic nucleator: 0.01～0.2.
Described acrylic resin is commercially available homo-polypropylene resin-oatmeal and commercially available crushing-resistant copolymerization acrylic resin powder.
The melt mass flow rate of described homo-polypropylene resin (MFR, 2.16kg, 230 ℃) is 5～20g/10min, and Mw/Mn is 3～7.
Described crushing-resistant copolymerization acrylic resin is the multipolymer of any one alpha-olefin in propylene and ethene, 1-butylene, 1-hexene or the 1-octene, wherein alpha-olefin content is 2～16mol%, melt mass flow rate (the MFR of crushing-resistant copolymerization acrylic resin, 2.16kg, 230 ℃) be 1～20g/10min, Mw/Mn is 4～8.
The preferred homo-polypropylene X30S powder of described homo-polypropylene resin-oatmeal, described crushing-resistant copolymerization acrylic resin powder preferred crushing-resistant copolymerization polypropylene QP73N powder and crushing-resistant copolymerization polypropylene QP83N powder.Crushing-resistant copolymerization polypropylene QP73N powder and crushing-resistant copolymerization polypropylene QP83N powder are produced by the Sinopec asphalt in Shenli Refinery, and homo-polypropylene X30S powder is produced by Dushanzi petro-chemical corporation.
Described thermo-stabilizer is Hinered phenols antioxidant or/and phosphite ester kind antioxidant, and the weight ratio of Hinered phenols antioxidant and phosphite ester kind antioxidant is 1: 0.1～10.
Described Hinered phenols antioxidant is: four [methyl-β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester, β-(3, the 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid, 1,3,5-trimethylammonium-2,4,6-three (3, the 5-di-tert-butyl-4-hydroxyl benzyl) benzene or 2,2-thiobis [3-(3,5-di-tert-butyl-hydroxy phenyl) ethyl propionate].
Described phosphite ester kind antioxidant is: three (2,4-di-tert-butyl-phenyl) phosphorous acid ester, two (2,4-DTBP) pentaerythritol diphosphites or diphosphorous acid tetramethylolmethane distearyl alcohol ester.
Described Metallic stearates is Zinic stearas or calcium stearate, preferred addition is 0.05～0.3 part, the effect of Metallic stearates is as the generation stearate that reacts of an acidic catalyst resistates in acid-acceptor and the acrylic resin, has simultaneously lubrication concurrently.
Described mineral filler is calcium carbonate, talcum powder, diatomite or mica, preferred calcium carbonate or talcum powder, and talcum powder most preferably, preferred addition is 0.1～0.3 part, inorganic filler particle is of a size of 0.01～50 μ m, preferred 0.1～10 μ m.
Described organic nucleator is phosphate metal salt nucleator, and preferred addition is 0.01～0.15 part.
The preferred nucleator HPN-68L of described phosphate metal salt nucleator, nucleant agent N A11 or nucleant agent N A21.The chemical name of nucleant agent N A11 is methylene-bis (2,4-di-tert-butyl-phenyl) phosphoric acid ester sodium, and the chemical name of nucleant agent N A21 is methylene-bis (2,4-di-tert-butyl-phenyl) phosphoric acid ester oxyaluminum salt.Nucleator HPN-68L is that Mei Liken chemical company produces, and nucleant agent N A11 and nucleant agent N A21 are that Ciba company produces.
The preparation method of polypropene composition of the present invention: each component with formula ratio mixes through mechanical mixer first, the stirring arm rotating speed is 500～2000rpm during mixing, then extrude through the twin-screw extruder melt blending, make after the granulation, prilling temperature is 160～250 ℃.
Beneficial effect of the present invention is as follows:
The present invention adopts composite mode to add a small amount of nucleator and a small amount of mineral filler when the granulation of acrylic resin powder, can meet or exceed modulus in flexure and the heat-drawn wire of adding the prepared acrylic resin of a large amount of nucleators, the polypropylene resin composite of making not only has high rigidity, height is heat-resisting, cost is low advantage, per ton cost reduces by 100～300 yuan, and can not improve the density of material, guaranteed the lightweight of goods.
Embodiment
Below in conjunction with embodiment the present invention is described further.
The melt mass flow rate MFR that relates in the present embodiment carries out according to GB/T 3682-2000, and experiment condition is load 2.16kg, 230 ℃ of temperature.Crushing-resistant copolymerization polypropylene QP73N powder and crushing-resistant copolymerization polypropylene QP83N powder are produced by the Sinopec asphalt in Shenli Refinery, and homo-polypropylene X30S powder is produced by Dushanzi petro-chemical corporation.
Embodiment 1
Embodiment 2
Embodiment 3
Embodiment 4
Embodiment 5
Embodiment 6
Embodiment 7
Embodiment 8
Embodiment 9
Embodiment 10
Comparative example 1
Comparative example 2
Comparative example 3
Comparative example 1～3 is corresponding with embodiment 2,7,9 prescription respectively, namely the prescription in except containing the acrylic resin consistent with corresponding Example formulations and consumption, thermo-stabilizer, stearate, do not add mineral filler, add the identical nucleator of corresponding prescription more than 1 times.
The preparation method of polypropene composition of the present invention: each component with formula ratio mixes through mechanical mixer first, rotating speed of agitator is 500～2000rpm during mixing, then extrude through the twin-screw extruder melt blending, make after the granulation, prilling temperature is 160～250 ℃.
Comparative example 1～3 and embodiment 2,7,9, rotating speed of agitator is 1000rpm during mixing, prilling temperature is 200 ℃; Embodiment 1, embodiment 3, embodiment 4, embodiment 5, embodiment 6, embodiment 8, embodiment 10, rotating speed of agitator is respectively 600rpm, 900rpm, 1800rpm, 1500rpm, 1200rpm, 800rpm, 1900rpm during mixing, and prilling temperature is respectively 245 ℃, 225 ℃, 205 ℃, 185 ℃, 215 ℃, 195 ℃, 165 ℃.
It is as shown in table 1 below that embodiment 1～10 and comparative example 1～3 product performance detect data.
Table 1 embodiment and comparative example product performance detect table
As can be seen from Table 1, the flexural strength of composition of the present invention, bending elastic modulus, load deformation temperature, Tc etc. have all reached the level of adding a large amount of nucleator resulting compositions, because the nucleator addition is few, therefore have cheaply advantage.
Claims (10)
1. polypropene composition is characterized in that being made by the raw material of following parts by weight:
2. polypropene composition according to claim 1 is characterized in that described acrylic resin is homo-polypropylene resin or crushing-resistant copolymerization acrylic resin.
3. polypropene composition according to claim 2, the melt mass flow rate that it is characterized in that described homo-polypropylene resin is 5～20g/10min, Mw/Mn is 3～7; Described crushing-resistant copolymerization acrylic resin is the multipolymer of any one alpha-olefin in propylene and ethene, 1-butylene, 1-hexene or the 1-octene, wherein alpha-olefin content is 2～16mol%, the melt mass flow rate of crushing-resistant copolymerization acrylic resin is 1～20g/10min, and Mw/Mn is 4～8.
4. polypropene composition according to claim 1 is characterized in that described thermo-stabilizer is Hinered phenols antioxidant or/and phosphite ester kind antioxidant, and the weight ratio of Hinered phenols antioxidant and phosphite ester kind antioxidant is 1: 0.1～10.
5. polypropene composition according to claim 4, it is characterized in that described Hinered phenols antioxidant is: four [methyl-β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester, the β-positive octadecanol ester of (3,5-di-tert-butyl-hydroxy phenyl) propionic acid, 1,3,5-trimethylammonium-2,4,6-three (3,5-di-tert-butyl-4-hydroxyl benzyl) benzene or 2,2-thiobis [3-(3,5-di-tert-butyl-hydroxy phenyl) ethyl propionate]; Described phosphite ester kind antioxidant is: three (2,4-di-tert-butyl-phenyl) phosphorous acid ester, two (2,4-DTBP) pentaerythritol diphosphites or diphosphorous acid tetramethylolmethane distearyl alcohol ester.
6. polypropene composition according to claim 1 is characterized in that described Metallic stearates is Zinic stearas or calcium stearate, and addition is 0.05～0.3 part.
7. polypropene composition according to claim 1 is characterized in that described mineral filler is calcium carbonate, talcum powder, diatomite or mica, and addition is 0.1～0.3 part, and inorganic filler particle is of a size of 0.01～50 μ m, preferred 0.1～10 μ m.
8. polypropene composition according to claim 1 is characterized in that described organic nucleator is phosphate metal salt nucleator, and addition is 0.01～0.15 part.
9. polypropene composition according to claim 8 is characterized in that described phosphate metal salt nucleator is nucleator HPN-68L, nucleant agent N A11 or nucleant agent N A21.
10. method for preparing the arbitrary described polypropene composition of claim 1～9, it is characterized in that: each component with formula ratio mixes through mechanical mixer first, the stirring arm rotating speed is 500～2000rpm during mixing, then extrude through the twin-screw extruder melt blending, make after the granulation, prilling temperature is 160～250 ℃.
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| CN103554660A (en) * | 2013-10-21 | 2014-02-05 | 中国石油化工股份有限公司 | High-rigidity high-heat-resistance homo-polypropylene material and preparation method thereof |
| CN103923381A (en) * | 2013-12-28 | 2014-07-16 | 上海普利特复合材料股份有限公司 | High-modulus and ultrahigh-impact polypropylene composite material and its preparation method |
| CN104562256A (en) * | 2014-12-31 | 2015-04-29 | 方文川 | Spinning-type polypropylene breaking elongation rate improving agent and preparation method thereof |
| CN105440455A (en) * | 2014-09-29 | 2016-03-30 | 中国石油化工股份有限公司 | Polypropylene composition, polypropylene material, use of polypropylene composition and drainpipe |
| CN105924769A (en) * | 2016-04-29 | 2016-09-07 | 三门峡中达化工有限公司 | Method for modifying polypropylene material with complex of phosphate salt and nano-material |
| CN106519445A (en) * | 2016-11-15 | 2017-03-22 | 华东理工大学 | High-rigidity heat-resistant polypropylene composite material and preparation method thereof |
| CN106893204A (en) * | 2016-07-17 | 2017-06-27 | 佛山瑞箭体育器材有限公司 | A kind of high rigidity polypropene composition |
| CN106905614A (en) * | 2016-07-20 | 2017-06-30 | 佛山瑞箭体育器材有限公司 | A kind of high rigidity polypropene composition |
| CN108239305A (en) * | 2016-12-27 | 2018-07-03 | 中国石油天然气股份有限公司 | A kind of toughening complex additive of acrylic resin and the preparation method of polypropylene anti-impact resin |
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| CN109535545A (en) * | 2018-10-22 | 2019-03-29 | 山东京博石油化工有限公司 | A kind of novel high just polypropylene modified material and preparation method thereof |
| CN109749397A (en) * | 2018-12-29 | 2019-05-14 | 上海日之升科技有限公司 | A kind of high shrinkage polyketone material and preparation method thereof |
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| CN112409681A (en) * | 2019-08-23 | 2021-02-26 | 中国石油化工股份有限公司 | Polypropylene composition and preparation method thereof |
| CN114437457A (en) * | 2021-12-08 | 2022-05-06 | 国家能源集团宁夏煤业有限责任公司 | Polypropylene material and preparation method and application thereof |
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| CN101942146A (en) * | 2009-07-10 | 2011-01-12 | 中国石油化工股份有限公司 | Controllable rheological high-gloss polypropylene resin and preparation method thereof |
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| CN105924769A (en) * | 2016-04-29 | 2016-09-07 | 三门峡中达化工有限公司 | Method for modifying polypropylene material with complex of phosphate salt and nano-material |
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| CN106519445A (en) * | 2016-11-15 | 2017-03-22 | 华东理工大学 | High-rigidity heat-resistant polypropylene composite material and preparation method thereof |
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