CN1300236C - Mineral/ whisker reinforced polypropylene composition - Google Patents
Mineral/ whisker reinforced polypropylene composition Download PDFInfo
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- CN1300236C CN1300236C CNB031159222A CN03115922A CN1300236C CN 1300236 C CN1300236 C CN 1300236C CN B031159222 A CNB031159222 A CN B031159222A CN 03115922 A CN03115922 A CN 03115922A CN 1300236 C CN1300236 C CN 1300236C
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- 239000004743 Polypropylene Substances 0.000 title claims abstract description 48
- -1 polypropylene Polymers 0.000 title claims abstract description 44
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 42
- 229910052500 inorganic mineral Inorganic materials 0.000 title claims abstract description 30
- 239000011707 mineral Substances 0.000 title claims abstract description 30
- 239000000203 mixture Substances 0.000 title claims abstract description 26
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 8
- 159000000003 magnesium salts Chemical class 0.000 claims abstract description 8
- 239000000654 additive Substances 0.000 claims abstract description 7
- 239000012744 reinforcing agent Substances 0.000 claims abstract description 7
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 6
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 6
- 239000003623 enhancer Substances 0.000 claims abstract description 5
- 238000002360 preparation method Methods 0.000 claims abstract description 5
- 239000007822 coupling agent Substances 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 8
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 6
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 238000001125 extrusion Methods 0.000 claims description 3
- 229920005629 polypropylene homopolymer Polymers 0.000 claims description 3
- 239000005995 Aluminium silicate Substances 0.000 claims description 2
- 235000012211 aluminium silicate Nutrition 0.000 claims description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 2
- 229920001577 copolymer Polymers 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims description 2
- 229920000578 graft copolymer Polymers 0.000 claims description 2
- 238000005469 granulation Methods 0.000 claims description 2
- 230000003179 granulation Effects 0.000 claims description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000000314 lubricant Substances 0.000 claims description 2
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 2
- 239000000155 melt Substances 0.000 claims description 2
- 239000010445 mica Substances 0.000 claims description 2
- 229910052618 mica group Inorganic materials 0.000 claims description 2
- 239000002530 phenolic antioxidant Substances 0.000 claims description 2
- 239000000049 pigment Substances 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims 1
- 239000012760 heat stabilizer Substances 0.000 claims 1
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 claims 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 5
- 238000001746 injection moulding Methods 0.000 abstract description 3
- 150000004291 polyenes Chemical class 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 239000002131 composite material Substances 0.000 description 4
- 230000002787 reinforcement Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000003017 thermal stabilizer Substances 0.000 description 1
- 239000012745 toughening agent Substances 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
本发明涉及一种矿物/晶须增强聚丙烯组合物，它配有聚内烯、矿物增强剂、增韧母粒、PP接枝相容剂、抗氧剂、其它助剂，其特点在于，加入晶须增强剂，本发明的制配方法是将除镁盐晶须之外的其他组分置于高混机中高速混合2～3分钟，加入镁盐晶须，低速混合1分钟左右，出料，然后将料在特殊螺杆组合的双螺杆机挤出造粒，双螺杆加工温度在170-240℃，螺杆转速在180-600转/分，本发明具有高强度、高刚度、抗冲击，并且尺寸稳定性好，横向纵向收缩率均匀，低翘曲等特点，适合于注塑成型仪表盘等汽车制件，也适合于注塑成型空调、洗衣机等家电用品。The invention relates to a mineral/whisker reinforced polypropylene composition, which is equipped with polyene, mineral reinforcing agent, toughening masterbatch, PP graft compatibilizer, antioxidant, and other additives, and is characterized in that: Add the whisker enhancer, the preparation method of the present invention is to put other components except the magnesium salt whisker in a high-speed mixer for 2 to 3 minutes at high speed, add the magnesium salt whisker, and mix at a low speed for about 1 minute, The material is discharged, and then the material is extruded and granulated in a twin-screw machine with a special screw combination. The twin-screw processing temperature is 170-240 ° C, and the screw speed is 180-600 rpm. The invention has high strength, high rigidity, and impact resistance. , and good dimensional stability, uniform horizontal and vertical shrinkage, low warpage, etc., suitable for injection molding of automotive parts such as instrument panels, and also suitable for injection molding of air conditioners, washing machines and other household appliances.
Description
技术领域technical field
本发明涉及一种矿物/晶须增强聚丙烯组合物，可用于车用制件、家电制件等，属于聚丙烯技术领域。The invention relates to a mineral/whisker reinforced polypropylene composition, which can be used for vehicle parts, home appliance parts, etc., and belongs to the technical field of polypropylene.
背景技术Background technique
聚丙烯作为一种通用塑料，它具有加工性能优良、机械性能好、耐化学腐蚀性等特点，在塑料中占有重要地位，但在制作工程部件时，其强度、刚度和耐热性远不能满足要求，同时聚丙烯冲击性能差，特别是低温冲击性能差，成型收缩率大，特别是纤维增强时纵横比收缩不均匀等缺点，这限制了聚丙烯在工程部件中的应用。As a general-purpose plastic, polypropylene has the characteristics of excellent processing performance, good mechanical properties, and chemical corrosion resistance. It occupies an important position in plastics, but its strength, stiffness, and heat resistance are far from satisfactory when making engineering components. At the same time, the impact properties of polypropylene are poor, especially at low temperature, and the molding shrinkage is large, especially the aspect ratio shrinkage is uneven when fiber is reinforced, which limits the application of polypropylene in engineering components.
欧洲专利EP-A496625公开一种高结晶聚丙烯的复合材料，其通过添加30％的滑石粉来达到高刚度的目的，但是这导致材料的冲击强度降低，从而限制了材料的应用，同时日本专利JP昭56-149318和日本专利JP昭61-256920、JP平4-36092介绍了制备镁盐晶须的方法，中国专利CN1288860A公开了一种新型镁盐晶须的制备方法，对其在高聚物，特别是在聚丙烯中的应用均没有涉及。European patent EP-A496625 discloses a composite material of high crystalline polypropylene, which achieves the purpose of high stiffness by adding 30% talcum powder, but this leads to a decrease in the impact strength of the material, thereby limiting the application of the material, while the Japanese patent JP Zhao 56-149318 and Japanese patent JP Zhao 61-256920, JP flat 4-36092 have introduced the method for preparing magnesium salt whisker, and Chinese patent CN1288860A discloses a kind of preparation method of novel magnesium salt whisker, to it in polymer Materials, especially in the application of polypropylene are not involved.
发明内容Contents of the invention
本发明的目的是提供一种具有高刚度、高强度、抗冲击并且收缩率低，横向纵向收缩率均匀，低翘曲的矿物/晶须增强聚丙烯组合物。The object of the present invention is to provide a mineral/whisker reinforced polypropylene composition with high rigidity, high strength, impact resistance, low shrinkage, uniform transverse and longitudinal shrinkage, and low warpage.
为实现以上目的，本发明的技术方案是提供一种矿物/晶须增强聚丙烯的组合物，其特征在于，它包括以下重量配比的原料制成：To achieve the above object, the technical solution of the present invention is to provide a composition of mineral/whisker reinforced polypropylene, which is characterized in that it comprises the following raw materials in weight ratio:
聚丙烯 50～60Polypropylene 50～60
矿物增强剂 15～35Mineral enhanced agent 15 ～ 35
晶须增强剂 4-15Whisker Enhancer 4-15
增韧母粒 15～30Rigid mother particles 15-30
PP接枝相容剂 3-10
抗氧剂 0.2～0.8Antioxidant 0.2 ～ 0.8
其它助剂 0.2～2.5Other additives 0.2～2.5
所述的聚丙烯可以是均聚聚丙烯、共聚聚丙烯，可以是单一的也可以是混合的，其熔融指数为5～25g/10min，拉伸强度≥20Mpa。The polypropylene can be homopolypropylene or copolymerized polypropylene, single or mixed, with a melt index of 5-25g/10min and a tensile strength of ≥20Mpa.
所述的矿物增强剂可以是云母、滑石粉、高岭土或者碳酸钙，其粒径为25μm～50μm。The mineral reinforcing agent can be mica, talcum powder, kaolin or calcium carbonate, and its particle size is 25 μm-50 μm.
所述的晶须增强剂为镁盐晶须，其长径比L/D≥30，粒径≤1μm。The whisker reinforcing agent is magnesium salt whisker, its aspect ratio L/D≥30, particle size≤1μm.
所述的增韧母粒为乙烯-辛烯共聚物(POE)橡胶，其熔融指数为0.4～5g/10min。The toughened masterbatch is ethylene-octene copolymer (POE) rubber, and its melt index is 0.4-5g/10min.
所述的PP接枝相容剂为聚丙烯与马来酸酐的接枝聚合物的低聚物，其熔融指数为40～100g/10min。The PP graft compatibilizer is an oligomer of graft polymer of polypropylene and maleic anhydride, and its melt index is 40-100g/10min.
所述的抗氧剂是一种受阻酚类抗氧剂，可以是四[β-(3，5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯。The antioxidant is a hindered phenolic antioxidant, which may be tetrakis[β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate] pentaerythritol ester.
所述的其它助剂可以是热稳定剂、润滑剂、抗紫外线剂或颜料。Said other additives can be thermal stabilizers, lubricants, anti-ultraviolet agents or pigments.
本发明的制备方法如下：The preparation method of the present invention is as follows:
(1)按配比秤取原料；(1) Take raw materials by weighing;
(2)将矿物表面经过偶联剂处理，这种偶联剂可以是硅烷偶联剂同系物或钛酸脂偶联剂同系物；(2) The mineral surface is treated with a coupling agent, which can be a silane coupling agent homolog or a titanate coupling agent homolog;
(3)将晶须表面经过偶联剂处理，这种偶联剂可以是硅烷偶联剂同系物或钛酸脂偶联剂同系物；(3) the whisker surface is treated with a coupling agent, which can be a silane coupling agent homologue or a titanate coupling agent homologue;
(4)将聚丙烯、矿物增强剂、增韧母粒、PP接枝相容剂、抗氧剂、其它助剂一起置于高混机中混合2-3分钟；(4) Put polypropylene, mineral reinforcement, toughening masterbatch, PP graft compatibilizer, antioxidant, and other additives together in a high-mixer and mix for 2-3 minutes;
(5)加入晶须增强剂低速混合1-2分钟；(5) Add whisker enhancer and mix at low speed for 1-2 minutes;
(6)出料；(6) Discharging;
(7)将混合的原料置于双螺杆机中挤出造粒，双螺杆机的转速为180-600转/分，温度为170-240℃。(7) Place the mixed raw materials in a twin-screw machine for extrusion granulation, the speed of the twin-screw machine is 180-600 rpm, and the temperature is 170-240°C.
本发明采用聚丙烯作为基体树脂，通过采用矿物/晶须复合增强技术，既解决了聚丙烯作为工程部件原料的刚度低、强度差、耐热性不高等缺陷，同时通过这种复合增强技术，结合增韧母粒，使材料的冲击强度大大提高，扩大了聚丙烯作为工程制件的应用领域，同时，矿物/晶须复合增强，解决了聚丙烯制品尺寸不稳定，横、纵收缩率不均匀的缺陷。The present invention uses polypropylene as the matrix resin, and adopts the mineral/whisker composite reinforcement technology, which not only solves the defects of polypropylene as a raw material for engineering parts, such as low stiffness, poor strength, and low heat resistance, but also through this composite reinforcement technology, Combined with the toughening masterbatch, the impact strength of the material is greatly improved, and the application field of polypropylene as engineering parts is expanded. At the same time, the mineral/whisker composite reinforcement solves the problem of unstable dimensions of polypropylene products and uneven horizontal and vertical shrinkage rates. Uniform defects.
本发明的优点是矿物/晶须增强聚丙烯具有高强度，高刚度，抗冲击、阻燃、尺寸稳定，适合于注射成型各类车用、家电用工程塑料件。The invention has the advantages that the mineral/whisker reinforced polypropylene has high strength, high rigidity, impact resistance, flame retardancy and stable size, and is suitable for injection molding various engineering plastic parts for vehicles and household appliances.
具体实施方案specific implementation plan
下面结合实施例，对本发明作进一步详细说明：Below in conjunction with embodiment, the present invention is described in further detail:
实施例1-4：Embodiment 1-4:
以共聚聚丙烯和均聚聚丙烯的共混物为基础料，以滑石粉/镁盐晶须为增强剂，PP-g-MAH为相容剂，POE橡胶母粒为增韧剂，其重量配比列于表1中，Based on the blend of copolymerized polypropylene and homopolypropylene, talcum powder/magnesium salt whisker is used as reinforcing agent, PP-g-MAH is used as compatibilizer, POE rubber masterbatch is used as toughening agent, its weight The ratio is listed in Table 1,
表一：矿物/晶须增强聚丙烯组合物组份的重量配比Table 1: Weight ratio of mineral/whisker reinforced polypropylene composition components
本发明的制备方法如下：The preparation method of the present invention is as follows:
(1)滑石粉经过偶联剂处理，；(1) talcum powder is treated with a coupling agent;
(2)将镁盐晶须表面经过偶联剂处理，；(2) the surface of the magnesium salt whisker is treated with a coupling agent;
(3)将聚聚丙烯、共聚聚丙烯、滑石粉、POE增韧母粒、PP接枝相容剂、抗氧剂1010一起置于高混机中混合3分钟；(3) Put polypropylene, copolymerized polypropylene, talcum powder, POE toughening masterbatch, PP graft compatibilizer, and antioxidant 1010 together in a high mixer and mix for 3 minutes;
(4)加入晶须镁盐晶须低速混合1分钟；(4) Add whisker magnesium salt whisker and mix at low speed for 1 minute;
(5)出料；(5) discharge;
(6)将混合的原料置于双螺杆机中挤出造粒，双螺杆机的转速为200转/分，双螺杆加工工艺列于表2中：(6) The mixed raw materials are placed in a twin-screw machine to extrude and granulate. The rotating speed of the twin-screw machine is 200 rpm, and the twin-screw processing technology is listed in Table 2:
表二：双螺杆挤出加工工艺Table 2: Twin-screw extrusion process
将粒料干燥注射成标准样条，测试性能，性能如表3：Dry and inject the pellets into a standard sample, and test the performance. The performance is shown in Table 3:
表三：矿物/晶须增强聚丙烯组合物性能测试对比Table 3: Performance test comparison of mineral/whisker reinforced polypropylene composition
对比实施例5-6：Comparative Examples 5-6:
对比不同滑石粉用量，其它组分作相应变化，其配比列于表4，其它操作与实施例1相同，测试性能列于表5：Contrast different talcum powder consumptions, and other components are changed accordingly, and its proportioning is listed in Table 4, and other operations are the same as in Example 1, and the test performance is listed in Table 5:
表四：矿物增强聚丙烯组合物的重量配比Table 4: Weight ratio of mineral reinforced polypropylene composition
将粒料干燥注射成标准样条，测试性能，性能如表：The pellets are dried and injected into a standard sample, and the performance is tested. The performance is shown in the table:
表五：矿物增强聚丙烯组合物性能测试对比Table 5: Performance Test Comparison of Mineral Reinforced Polypropylene Compositions
Claims (9)
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| CN104312006A (en) * | 2014-09-24 | 2015-01-28 | 雪龙集团股份有限公司 | Reinforced wear-resistant polypropylene composite material |
| CN105111585A (en) * | 2015-09-10 | 2015-12-02 | 常州塑金高分子科技有限公司 | Polypropylene washing machine powder filling granules for recovery and preparation method thereof |
| CN109337199A (en) * | 2018-09-14 | 2019-02-15 | 君恒咨询有限公司 | A kind of polypropylene building mould additive and preparation method thereof |
| CN110092926A (en) * | 2019-06-11 | 2019-08-06 | 吕智 | The preparation method and applications of alkali magnesium sulfate crystal whisker master batch |
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| EP0496625A2 (en) * | 1991-01-25 | 1992-07-29 | Mitsubishi Chemical Corporation | Thermoplastic polymer composition |
| US6150442A (en) * | 1998-12-31 | 2000-11-21 | Ferro Corporation | Flame retardant polypropylene composition |
| CN1328084A (en) * | 2001-07-03 | 2001-12-26 | 成都市华硕实业有限公司 | Composite of microfibre, superfine powder and polypropylene |
-
2003
- 2003-03-21 CN CNB031159222A patent/CN1300236C/en not_active Expired - Lifetime
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0496625A2 (en) * | 1991-01-25 | 1992-07-29 | Mitsubishi Chemical Corporation | Thermoplastic polymer composition |
| US6150442A (en) * | 1998-12-31 | 2000-11-21 | Ferro Corporation | Flame retardant polypropylene composition |
| CN1328084A (en) * | 2001-07-03 | 2001-12-26 | 成都市华硕实业有限公司 | Composite of microfibre, superfine powder and polypropylene |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1532221A (en) | 2004-09-29 |
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