CN101182381A - Polypropylene modified material and preparation method thereof - Google Patents
Polypropylene modified material and preparation method thereof Download PDFInfo
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- CN101182381A CN101182381A CNA2007100469090A CN200710046909A CN101182381A CN 101182381 A CN101182381 A CN 101182381A CN A2007100469090 A CNA2007100469090 A CN A2007100469090A CN 200710046909 A CN200710046909 A CN 200710046909A CN 101182381 A CN101182381 A CN 101182381A
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Abstract
The invention belongs to the technological field of polymer material and in particular relates to a modified polypropylene material and a preparation method thereof. The material at least consists of a polypropylene-based polymer matrix and a beta nucleater; other wear-resistant modifiers and various auxiliary agents (such as processing aid, antioxidant, coloring agent) can also be added. The invention is characterized in that the polypropylene matrix comprises a beta crystal, which means that the polypropylene crystals in the matrix material can be transformed from conventional alpha crystals partly or totally into beta crystals. The preparation method is usually the extruding method, the molding method or the injection method; the beta nucleater can be made into master batch for addition or be directly added; the beta nucleater can be added before the polymerization of polymers or after the polymerization and before the extrusion and granulation. Compared with the usual polypropylene materials of the alpha crystals, the wear rate of the wear-resistant material produced in the invention is reduced by more than 30 percent; and the wear-resistant material usually has better toughness and a higher heat distortion temperature.
Description
Technical field
The invention belongs to technical field of polymer materials, it is material modified and preparation method thereof to be specifically related to a kind of wear-resisting polypropene.
Background technology
Polypropylene (Polypropylene, abbreviation PP) is little because of having density, and electrical property, erosion resistance, wholesomeness, humidity resistance is good and advantage such as good processability and obtain widespread use.But also there are shortcomings such as easy to wear in PP, and its wear rate is higher than materials such as polyethylene far away.Drawbacks limit easy to wear PP in wide field more particularly as the application of engineering materials in high-end fields such as automobile, manufacturing, building, chemical pipelines.PP is carried out the high performance study on the modification, reduce its wear rate, thereby its application extension is arrived more wide field, have important practical significance.
At present, the main method of improving the polymer materials wear resistance is to add the high abrasion filler, as materials such as moly-sulfide, boron nitride, CNT (carbon nano-tube), tetrafluoroethylene, thereby improves the wear resistance of body material.By this method, realized modification to multiple macromolecular material.But,, but still can not satisfy the needs of practical application although also can improve its wear resistance by this method because the wear resistance of PP matrix own is too poor.
PP is as a kind of semi-crystalline polymer of high-crystallinity, and crystal property is determining its physical and mechanical properties to a certain extent.The molecule of isotatic polypropylene can form multiple crystalline structure such as α, β, γ, δ and plan six side's attitudes under different condition.(α-PP), the PP of this crystal formation itself just has the not high characteristics of poor toughness, temperature classification, and this also is the reason of common PP erosion-resisting characteristics difference all to form alpha-crystal form at common processing conditions.Beta crystal on the thermodynamics be metastable, be to be unfavorable for a kind of crystal formation of generating on kinetics, but the PP of this crystal formation (β-PP) has excellent impact property (notched Izod impact strength surpasses α-PP several times) and resistance toheat (heat-drawn wire is higher more than 20 ℃ than α-PP).If can induce the what is called " beta nucleater " that generates beta crystal by adding some, the crystal formation of matrix PP in the inorganic modified material is become the content of β type or raising beta crystal, might overcome then that common PP toughness of material is poor, temperature classification not high " bottleneck " problem, make the PP matrix material realize strengthening simultaneously toughness reinforcing and further improve the purpose of temperature classification.But,,, mainly concentrate on the research of physical and mechanical properties aspects such as mechanical property, resistance toheat, and its wearing character aspect has not been seen any bibliographical information as yet for the research of β-PP up till now for extremely.
We discover recently, compare with common α-PP, and β-PP has the wear rate of obvious reduction.Core content of the present invention is promptly based on this characteristic of β-PP: if the crystal habit of PP partly or entirely is transformed into beta crystal, then can improve the wear resistance of PP sill.
Since the beta crystal of PP on the thermodynamics be metastable, be to be unfavorable for a kind of crystal formation of generating on kinetics, under common processing or crystallization condition, be difficult to obtain, only (as in certain thermograde, or shearing action) could form under special conditions.Add some can induce the what is called " beta nucleater " that generates beta crystal but be can obtain the high-content beta crystal, also be the approach of unique industrializing implementation at present.The beta nucleater that has obvious β crystallization effect at present or produce considerable influence in this field mainly contains the γ quinacridone that Leugering finds (the dyestuff E3B of γ-Quinacridone), the mixture of the salt of some IIa family element or itself and specific di-carboxylic acid (typical example is calcium stearate/pimelic acid mixture or pimelic acid calcium), aryl amide nucleator and rare earth beta nucleater etc.No matter but be which kind of method, or use which kind of nucleator, as long as can improve the content of beta crystal among the PP, just can be used for improving the wear resistance of this material.
Along with developing rapidly of industries such as China's household electrical appliances, automobile, material of construction, the material modified demand of various high-grade PP will sharply increase.Improve the wear resistance of PP material and correlated product, the application extension of PP to some field that engineering plastics or other high performance material are in the past used, is not only had very huge economic benefit, have the important social benefit simultaneously.
Summary of the invention
The object of the present invention is to provide a kind of excellent abrasive resistance polypropylene modified material and preparation method thereof that has.
Polypropylene modified material proposed by the invention, its principal feature are to contain a certain proportion of beta crystal among the matrix PP.This beta crystal can be to obtain by the control processing conditions, also can be to obtain by adding beta nucleater.By certain thermograde, or crystallization under effects such as shearing, pressure, a certain proportion of beta crystal can be obtained.But method more commonly used is to obtain a certain proportion of beta crystal by the method that adds beta nucleater.
Therefore, polypropylene modified material proposed by the invention is made up of following two kinds of components: polypropylene matrix material, beta nucleater at least.Make and contain beta crystal in the polypropylene matrix material but usually need add that other is material modified,, particularly can also use other to be used to improve the material of wear resistance as processing aid, dispersion agent, oxidation inhibitor, toughener, toughner, tinting material or the like toward contact.
It is all material of base resin that described polypropylene matrix material is meant with the polypropylene, comprises with polypropylene being the mixture of main matrix, waits until as polypropylene composite material, polypropylene alloy.And described base resin is meant various polypropylene.Comprising homo-polypropylene (PP-H), block copolymerization polypropylene (PP-B), atactic copolymerized polypropene (PP-R), also can be various polyacrylic mixtures, or the mixture formed of polypropylene and other polymer or other material.
Nucleator among the present invention, it can be any material that can induce PP to form beta crystal, comprise a few class beta nucleaters commonly used at present, as the fused ring compound class with directrix plane structure is (as γ quinacridone γ-Quinacridone dyestuff, triphen dithiazine Triphenodithiazine etc.), the mixture of the salt of some IIa family element or itself and specific di-carboxylic acid or compound are (as calcium stearate/pimelic acid mixture, pimelic acid calcium etc.), aromatic amides class (as phthalic acid Cyclohexamide and naphthalic acid Cyclohexamide etc.) beta nucleater, and the rare earth beta nucleater etc.Can be a certain independent use, also can be the mixture of several and usefulness.The consumption of nucleator is generally 0.0001%-10% (quality) with respect to the polypropylene in the matrix, is preferably 0.0002%-3% (quality).
The present invention improves the method for polypropylene-base material wear resistance, can combine with the method for the raising wear resistance that generally adopts at present, to give the material better wear resistance.As when adding beta nucleater, add the material that other can improve material wear ability, as wear-resisting properties-correcting agent such as moly-sulfide, boron nitride, CNT (carbon nano-tube).Promptly when forming beta crystal, combine with the method for the raising wear resistance that generally adopts at present, with the wear resistance of further raising material.
In the material of the present invention, also can use various other auxiliary agents according to the actual requirements, as processing aid, dispersion agent, oxidation inhibitor, tinting material, filler etc.
Several main components composition (mass parts) ratios are as follows among the present invention:
Polypropylene is 100 parts in the matrix
Beta nucleater 0.0001-10 part
Other wear-resisting properties-correcting agent 0-100 part
The preparation method who uses among the present invention is general polymer modification or product processing method, as extrude, mold pressing, injection etc., do not have particular requirement.Beta nucleater can be distributed in the macromolecule matrix with the Process Technology of Polymer method of routine, as makes master batch and add matrix, directly add matrix, also can before polymerization, add on the synthesizer with catalyzer, or after polymerization, add before the extruder grain etc.
By polypropylene modified material provided by the invention, its wear resistance has great improvement than matrix, cooperate again with other original use always material modified, as add the material of processing aid commonly used, oxidation inhibitor, toughener, toughner and other modified abrasion resistant, polypropylene modified material that can the obtained performance excellence, thus the polypropylene material Application Areas can be expanded greatly.
Embodiment
By the following examples the present invention is further described, wherein form umber, content all by weight.
Embodiment 1
100 parts of polypropylene (trade mark F401, melt body flow rate 2.5g/10min, density 0.91g/cm3) mixing with two roller mills in 170 ℃, the plasticizing back adds 0.5 part of rare earth beta nucleater, sheet under behind the mixing 3min, be molded into the thick sheet material of 6mm with vulcanizing press in 190 ℃ then, note is made sample P P-1.Utilize omnipotent sampling machine, make the sample of specification for height * wide * length=6mm * 7mm * 30mm.As a comparison, pure PP F401 also makes batten with same process, and note is made prescription PP-0.
Cut 5-10mg from sample surfaces, utilize Perkin-Elmer DSC-7 thermal analyzer (DSC), N
2Protection is heated to 200 ℃ with the scanning speed of 10 ℃/min from room temperature, and constant temperature 5min is cooled to 30 ℃ with 10 ℃/min speed after eliminating thermal history, and the scanning speed with 10 ℃/min is heated to 200 ℃ again, and the record sample is melting process for the second time.Near T 154 ℃
1The melting peak that the place occurs is the brilliant melting peak of β, and heat content is Δ H
β, near T 167 ℃
2The melting peak that the place occurs is the brilliant melting peak of α, and heat content is Δ H
α, the relative content of beta crystal is calculated by following formula (1),
k
DSC＝ΔH
β/(ΔH
α+ΔH
β) (1)
The relative content of beta crystal often also by wide-angle x-ray diffraction (WAXD), utilizes following Turner-Jones formula (2) to try to achieve simultaneously:
k
x＝H
β1/(H
β1+H
α1+H
α2+H
α3) (2)
H
α 1, H
α 2, H
α 3Be the height at the peak of three strong diffraction peaks (110) relevant on the wide-angle x-ray diffractogram, (040) and (130) with alpha-crystal form, H
β 1It is the height of beta crystal (300) diffraction peak.The beta crystal relative content sees Table 1 in the measured sample.
Table 1 different ingredients each crystal formation content and crystallization rate
| Prescription | T1(℃) | T 2(℃) | k DSC(％) | k x(％) | k(mm 3/N.m) |
| PP0 PP-1 | Do not have 154.3 | 168.0 167.5 | 0 69 | 0 88 | 2.3 1.5 |
Above-mentioned sample carries out the friction and wear behavior test on M-2000 type wear testing machine (friction pair is the steel annulus, and it is the 45# steel loop of 45mm that the antithesis test ring adopts external diameter.Test temperature is a room temperature, and humidity is 50 ± 10%, and slip speed is 0.42m/s, load 100N), the wear volume (mm of sample
3) and wear rate (mm
3/ N.m) calculate by following formula:
Wherein v is the sample wear volume, and l is the sample width, and r is the steel loop radius, and b is sample wearing and tearing width.The wear rate k of two kinds of samples also lists in table 1.As can be seen, the system wear rate behind the adding rare earth beta nucleater reduces about 34%.
Embodiment 2
Other is with embodiment 1, the rare earth beta nucleater mixes with PP earlier, making beta nucleater content by two roller mills is 5% master batch, above-mentioned master batch is with 5% consumption and PP mix particles, behind the twin screw extruder mixing granulation, be prepared into the sample that specification is height * wide * length=6mm * 7mm * 30mm with injection moulding machine.Measure its wear rate, find that the sample contain beta nucleater compares with the sample that does not contain beta nucleater, wear rate descends about 32%.Simultaneously, mechanical property and resistance toheat test shows are compared with unmodified PP, and the simply supported beam notched Izod impact strength of matrix material has improved 80%, and heat-drawn wire has improved 12C ℃.
Embodiment 3
Other is with embodiment 1, wherein the matrix homo-polypropylene change into block copolymerization polypropylene (trade mark is EPS30RF, melt flow rate (MFR) 2.6g/10min (230 ℃, 2.16kg), after tested, the gained material is compared with unmodified, wear rate descends about 38%.
Embodiment 4
Other is with embodiment 1, and wherein beta nucleater is not the rare earth nucleator, but the naphthalic acid Cyclohexamide, after tested, the gained material is compared with unmodified, and wear rate reduces about 30%.
Embodiment 5
(trade mark F401 melts body flow rate 2.5g/10min, density 0.91g/cm to 100 parts of polypropylene
3) and 20 parts of boron nitride, 2 parts of rare earth beta nucleaters, in the sheet pelletizing down of mixing even back, be molded into the thick sheet material of 6mm with vulcanizing press in 190 ℃ with two roller mills then, utilize omnipotent sampling machine, make the sample of specification, measure its polishing machine for height * wide * length=6mm * 7mm * 30mm.The gained material is compared with unmodified body material, and wear rate descends about 67%.
Embodiment 6
Other is with embodiment 5, but will be wherein 20 parts of 20 parts of boron nitride be changed to the mixture of 10 parts of boron nitride and 10 parts of tetrafluoroethylene.After tested, the gained material is compared with unmodified body material, and wear rate descends about 75%.
Embodiment 7
Other is with embodiment 5, but wherein 100 parts of polypropylene of matrix are changed to the mixture of 80 parts of PP and 20 parts of polyamide 66s.After tested, the gained material is compared with the PP/PA66 mixture that consisted of 80: 20, and wear rate descends about 51%.
Embodiment 8
Other is with embodiment 1, and wherein beta nucleater is not the rare earth nucleator, but consists of calcium stearate/pimelic acid mixture of 1: 1, and after tested, the gained material is compared with unmodified, and wear rate reduces about 30%.
Embodiment 9
The PP that handles with the material modified and non-modified among the embodiment 2 extrudes the sheet material that thickness is 2mm respectively, and cut with lathe, find that sheet material tweeting sound when machining that modifying material produces is lighter, and the sheet material that unmodified PP produces adds and sends ear-piercing sharp tweeting sound man-hour.
Embodiment 10
Measure mechanical property and the resistance toheat of the PP of the material modified and non-modified processing among the embodiment 5, compare with unmodified PP, the simply supported beam notched Izod impact strength of matrix material has improved 30%, and heat-drawn wire has improved 26 ℃.
Claims (7)
1. polypropylene modified material, it is characterized in that obtaining by polypropylene matrix material and two kinds of raw material preparing of beta nucleater at least, make in the polypropylene matrix material and form beta crystal, the consumption of beta nucleater is the 0.0001%-10% of polypropylene weight in the polypropylene matrix material; Wherein:
It is the material of base resin that described polypropylene matrix material is meant with the polypropylene, and base resin is meant various polypropylene.
2. polypropylene modified material according to claim 1 is characterized in that described is that the material of base resin comprises polypropylene composite material, polypropylene alloy with the polypropylene.
3. polypropylene modified material according to claim 1 is characterized in that the polypropylene in the described polypropylene matrix material is homo-polypropylene, block copolymerization polypropylene, atactic copolymerized polypropene, or the mixture of different materials in these polypropylene.
4. polypropylene modified material according to claim 1 and 2, it is characterized in that described beta nucleater is γ quinacridone, triphen dithiazine, calcium stearate/pimelic acid mixture, pimelic acid calcium, perhaps being aromatic amides class beta nucleater, perhaps is the rare earth beta nucleater.
5. polypropylene modified material according to claim 1 and 2 is characterized in that also being added with in the material in the moly-sulfide that can improve material wear ability, boron nitride, the CNT (carbon nano-tube) one or more, and add-on is below 100% of polypropylene quality.
6. polypropylene modified material according to claim 1 and 2 is characterized in that in the material also adding that processing aid, dispersion agent, oxidation inhibitor, tinting material, filler are arranged.
7. the preparation method of a polypropylene modified material as claimed in claim 1, it is characterized in that adopting conventional polymer modification or product processing method, comprise extrusion molding, compression molding or injection, beta nucleater is made master batch and is added in the body material, perhaps directly add in the polypropylene matrix material, perhaps before polymerization, adding on the synthesizer, perhaps after polymerization, adding before the extruder grain with catalyzer.
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| CN102040778A (en) * | 2010-12-24 | 2011-05-04 | 金发科技股份有限公司 | High-filling high-heat distortion temperature polypropylene composite material and preparation method thereof |
| CN102093637A (en) * | 2011-01-20 | 2011-06-15 | 南昌天高新材料股份有限公司 | Method for preparing beta nucleating agent modified polypropylene geogrid |
| CN102160506A (en) * | 2010-12-24 | 2011-08-24 | 内蒙古普力司达体育设施工程有限公司 | Salt retaining plate |
| CN102516640A (en) * | 2011-11-18 | 2012-06-27 | 武汉金牛经济发展有限公司 | Production technology for polypropylene tubing containing beta crystal form |
| CN102604211A (en) * | 2012-02-25 | 2012-07-25 | 美的集团有限公司 | Impact-resistant weather-resistant polypropylene material for lamps and manufacturing method thereof |
| CN102720896A (en) * | 2012-06-11 | 2012-10-10 | 杭州恒标管业有限公司 | Pipe as well as preparation method and purpose of pipe |
| CN101735512B (en) * | 2009-12-28 | 2013-04-17 | 上海金发科技发展有限公司 | Beta-crystalline homopolymerization polypropylene composition for inner chamber of water heater and preparation method thereof |
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| CN103146061A (en) * | 2013-03-15 | 2013-06-12 | 东风(十堰)非金属部件有限公司 | Rare-earth modified master batch for polypropylene and preparation method thereof |
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| CN113136074A (en) * | 2021-04-23 | 2021-07-20 | 宁夏永润新材料科技有限公司 | High-toughness homo-polypropylene composition and preparation method thereof |
| CN114395193A (en) * | 2022-03-04 | 2022-04-26 | 安徽飞达电气科技有限公司 | Polypropylene film and preparation method thereof |
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| CN101735512B (en) * | 2009-12-28 | 2013-04-17 | 上海金发科技发展有限公司 | Beta-crystalline homopolymerization polypropylene composition for inner chamber of water heater and preparation method thereof |
| CN102160506A (en) * | 2010-12-24 | 2011-08-24 | 内蒙古普力司达体育设施工程有限公司 | Salt retaining plate |
| CN102040778B (en) * | 2010-12-24 | 2012-07-11 | 金发科技股份有限公司 | High-filling high-heat distortion temperature polypropylene composite material and preparation method thereof |
| CN102040778A (en) * | 2010-12-24 | 2011-05-04 | 金发科技股份有限公司 | High-filling high-heat distortion temperature polypropylene composite material and preparation method thereof |
| CN102093637A (en) * | 2011-01-20 | 2011-06-15 | 南昌天高新材料股份有限公司 | Method for preparing beta nucleating agent modified polypropylene geogrid |
| CN102093637B (en) * | 2011-01-20 | 2012-11-28 | 南昌天高新材料股份有限公司 | Method for preparing beta nucleating agent modified polypropylene geogrid |
| CN102516640A (en) * | 2011-11-18 | 2012-06-27 | 武汉金牛经济发展有限公司 | Production technology for polypropylene tubing containing beta crystal form |
| CN102516640B (en) * | 2011-11-18 | 2013-05-01 | 武汉金牛经济发展有限公司 | Production technology for polypropylene tubing containing beta crystal form |
| CN102604211A (en) * | 2012-02-25 | 2012-07-25 | 美的集团有限公司 | Impact-resistant weather-resistant polypropylene material for lamps and manufacturing method thereof |
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| CN103073793A (en) * | 2013-01-09 | 2013-05-01 | 四川大学 | High-strength and high-toughness polypropylene pipe and preparation method thereof |
| CN103073793B (en) * | 2013-01-09 | 2015-06-24 | 四川大学 | High-strength and high-toughness polypropylene pipe and preparation method thereof |
| CN103087422A (en) * | 2013-02-19 | 2013-05-08 | 复旦大学 | Random copolymerization polypropylene modified material |
| CN103146061A (en) * | 2013-03-15 | 2013-06-12 | 东风(十堰)非金属部件有限公司 | Rare-earth modified master batch for polypropylene and preparation method thereof |
| CN105419107A (en) * | 2016-01-11 | 2016-03-23 | 宁波高新区辉门科技有限公司 | Bearing type foot pad plastic for instrument and preparation method thereof |
| CN106243510A (en) * | 2016-08-29 | 2016-12-21 | 合肥会通新材料有限公司 | A kind of high abrasion modified polypropylene composite material and preparation method thereof |
| CN109627591A (en) * | 2018-12-25 | 2019-04-16 | 金旸（厦门）新材料科技有限公司 | A kind of high antimicrobial form polypropylene modified material of soft sense of touch and preparation method thereof |
| CN112625349A (en) * | 2020-12-16 | 2021-04-09 | 广州华新科智造技术有限公司 | Wear-resistant master batch for polypropylene spinning material and preparation method thereof |
| CN113136074A (en) * | 2021-04-23 | 2021-07-20 | 宁夏永润新材料科技有限公司 | High-toughness homo-polypropylene composition and preparation method thereof |
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