CN103454303A - Rapid method for evaluating processing linear velocity of special-purpose material for biaxially oriented polypropylene - Google Patents
Rapid method for evaluating processing linear velocity of special-purpose material for biaxially oriented polypropylene Download PDFInfo
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Abstract
The invention relates to a rapid method for evaluating processing linear velocity of a special-purpose material for biaxially oriented polypropylene (BOPP). A thermal fractionation technology is employed to detect the chain structure distribution of the special-purpose material for BOPP, so as to obtain a differential scanning calorimetry curve of the special-purpose material after continuous self-seeding nucleation thermal fractionation; and a ratio of the height of a first melting peak to that of a second melting peak is read from the differential scanning calorimetry curve, or an area ratio of the two melting peaks is calculated through integration. If the ratio of peak height or peak area is no higher than 2, the special-purpose material has processing linear velocity higher than 420 m / min and is applicable to high speed processing; and if the ratio of peak height or peak area is larger than 2, the special-purpose material has processing linear velocity lower than 420 m / min and is applicable to relative low speed processing. The method provided by the invention is rapid and convenient, has accuracy and validity, can accelerate research and development process of a novel BOPP product, and is suitable for BOPP manufacturers to carry out raw material screening and quality control.
Description
Technical field
The present invention relates to the evaluation method of the processing characteristics of a kind of Biaxially oriented polypropylene (BOPP) PP Pipe Compound.But especially BOPP PP Pipe Compound processing line speed a kind of fast and the effectively evaluating method.
Background technology
Biaxially oriented polypropylene (BOPP) film, be acrylic resin by extruding curtain coating, vertically and horizontally stretching, being subject to the processes such as thermal finalization, produce film.Because the BOPP film has passed through biaxial orienting, laterally, mechanical property is good longitudinally, intensity is large, gas barrier property is high, good, the printing performance of the transparency and tear resistance are good, be the kind of consumption maximum in the PP film article, be widely used in packaging for foodstuff, medical package, industrial packaging and tobacco package etc.Up to the present, domestic construction tens the BOPP production lines of having gone into operation, a lot of petrochemical industry polypropylene plants both domestic and external are being produced the BOPP PP Pipe Compound.
The key technical index of BOPP PP Pipe Compound is melt flow rate and isotacticity.Isotacticity is higher.Crystallinity is higher, and high-regularity often makes PP Pipe Compound produce the rupture of membranes phenomenon when stretching.The low strength decreased that can cause film of isotacticity, deflection descends, and produces adhesion.Normal BOPP PP Pipe Compound is controlled between 94～97%.Melt flow rate (MFR) has reflected the mobility of melt.MFR is lower shows that the average relative molecular mass of PP Pipe Compound is higher, and melt viscosity is higher, can cause PP Pipe Compound processing unstable, causes that thickness fluctuation is large.Melt flow rate is higher, and the PP Pipe Compound extrusion flowability is good, but curtain coating forms the stretching poor ductility of slab, so the melt flow rate of BOPP PP Pipe Compound is controlled at 2.8～3.2g/min.
Along with the increase of domestic BOPP film demand and the development of multi-layer co-extruded technology, BOPP processing film technology is to the future development of high linear speed, high yield, so the adaptable process velocity of the PP Pipe Compound of BOPP receives much concern.What restrict BOPP PP Pipe Compound process velocity is mainly drawing process, and slab at a certain temperature, is carried out longitudinal stretching, and the spherocrystal melting in molecule is subject to detrusion simultaneously, and in spherocrystal, platelet melting solution twines, stretch orientation.Line speed improves and to require the platelet melting to accelerate, and makes the molecule activity ability strengthen, and is convenient to orientation, otherwise or cause intermolecular orientation movement inhomogeneous, cause rupture of membranes.At a certain temperature, lamellae thickness is thicker.Melting needs heat more, and melting speed is slower, more easily causes the generation of brilliant point and rupture of membranes.In actual molding is produced, the situation that the BOPP raw material of each family is close with isotacticity in melt flow rate, but there is notable difference in the processing characteristics of PP Pipe Compound.This is because conventional sense physical quantity melt flow rate and isotacticity are all average physical quantitys.In the situation that isotacticity is identical, the isotacticity of PP Pipe Compound distributes but not identical, and there is polydispersity in its distribution.The polydispersity that isotacticity (crystallizable isotactic sequence) distributes shows that processing and forming and usability with close or identical copolymerization composition sample have significant difference.Therefore, the polydispersity of this micromechanism makes PP Pipe Compound at melt flow rate and isotacticity, or even molecular weight is all in identical situation, and there is notable difference in the processability of PP Pipe Compound.The study general of polyolefin sequences structure is all first classification, then the micromechanism of each fraction is studied.Stage division comprises the classification of solvent gradient [Cai H, Luo X, Ma D, Wang J, Tan H.J Appl Polym Sci, 1999,71:93; Urdampilleta I, Gonz á lez A, Iruin J J, de la Cal J C, Asua J M.Macromolecules, 2005,38:2795], temperature rising elution classification and intersect classification [Nakatani H, Manabe N, Yokota Y, Minami H, Suzuki S, Yamaguchi F, Terano M.Polym Int, 2007,56:1152].This stage division is very effective to the distribution that characterizes crystalline sequence and be distributed between strand, but length consuming time of this several method, and cost is high, is difficult for promoting on a large scale.The micromechanism of each fraction that classification obtains is studied as stereoregularity adopts nuclear-magnetism carbon spectrum and infrared spectroscopy method usually.Nuclear-magnetism carbon spectral method is ripe, accuracy is high, but its testing cost is also high, and it can not distinguish the distribution of the segment sequence that surpasses 5 unit, makes the limitation of the method also apparent in view.Analyze the spatial structure sequence or or the length of chemical composition sequence, existing infrared spectrum is sent out the length that also can only determine more than 10 main chain carbons.Therefore, be necessary to develop a kind of simple and easy to do, can evaluate and test cheaply a kind of method of crystallizable sequence.
Hot classification technique development based on differential scanning calorimeter starts from 19th-century seventies.But hot classification technique is a kind of new technology of a kind of molecular chain structure via well-designed thermal cycle testing procedure rapid evaluation thermoplasticity those semi-crystalline materials heterogeneous (chain heretogeneities) degree.This new technology is especially effective to short-chain branched degree and the short-chain branched distribution of investigating ethylene/alpha-olefin copolymer.Wherein, continuously spontaneous nucleation hot classification (SSA) technical development of annealing starts from 19th-century nineties, is a kind of ageing a kind of Novel hot classification technique that development potentiality is more arranged that has more.The SSA technology is based on a kind of of means of differential scanning calorimetry equipment a series of spontaneous nucleation and annealing steps is applied to a kind of hot stage division on macromolecule sample.Nearly decades, due to DSC equipment have easy and simple to handle, amount of samples is few, the advantage such as short consuming time, the hot classification technique based on DSC is obtained develop rapidly, is tending towards gradually ripe.The multiple melting peaks that hot classification obtains after processing is corresponding from the segment of different crystallizable sequence lengths, and the different chips thickness of the segment of different crystallizable sequence lengths and the degree of branching and formation is corresponding one by one.The size of the integral area of the multiple melting peaks curve how many available heat classifications of the content of corresponding segment obtain after processing quantizes.Hot classification technique has been widely used in investigating short-chain branched degree and the short-chain branched distribution of linear low density polyethylene.Current hot classification technique is used main pooled applications on ethylene/alpha-olefin copolymer, and the polypropylene sequence is distributed to study rarely has report.The crystallizable isotactic sequence that Kravchenko had once studied with hot classification technique the polypropylene elastomer that isotaxy five-tuple sequence mmmm content is 25% and 30% distribute [Kravchenko R A, Sauer BB, Scott McLean R, et al.Macromolecules, 2000,33,11-13].Wang Dujin had once studied inhomogeneity [the Zhu H of the composition of two kinds of polypropylene reaction alloys (ethylene-co-butylene polypropylene and ethylene-co-propylene polypropylene) with hot classification technique, Monrabal B., Han C C, Wang D. Macromolecules, 2008,41:826-833].We are incorporated into by hot classification technique the mensuration that the crystallizable sequence of BOPP distributes, effectively but the processing line speed combination of its crystallizable isotactic sequence distributional difference and BOPP is got up, by detect the crystallizable sequence of BOPP distribute (wafer thickness distributions) but estimate PP Pipe Compound processing line speed method just.The method is very suitable for being used as petroleum chemical enterprise or its BOPP manufacturing enterprise carry out the quality testing of BOPP PP Pipe Compound and evaluation a kind of effective hand means fast.
Summary of the invention
A kind of method that the purpose of this invention is to provide Fast Evaluation BOPP special materials processing line speed.By the test analysis to the crystallizable isotactic sequence distribution of resin and aggregated structure, the BOPP PP Pipe Compound is carried out to conveniently processing characteristics evaluation and quality control.The test analysis that the crystallizable sequence of resin distributes and the aggregated structure wafer thickness distributes is applied continuous spontaneous nucleation hot classification (SSA) technology of annealing and is completed at differential scanning calorimeter.This test specific procedure is set reference literature [Arnal, M.L.; Sanchez, J.J.; Muller, A.J.Polymer 2001,42,6877-6890].Illustrate the program setting on differential scanning calorimeter: a. and sample is warming up to high temperature (guaranteeing that the abundant melting of sample gets final product) constant temperature a period of time under nitrogen protection to eliminate thermal history; B. sample is down to low temperature (be generally 0～50 ℃, sample sample is crystallizable at this temperature get final product) with certain rate of temperature fall, and at this temperature constant temperature a period of time in order to set up the standard thermal history of sample; C. sample is risen to a spontaneous nucleation temperature T set with certain heating rate
s, and constant temperature a period of time (1～30min); D. repeating step b; E. sample is risen to next spontaneous nucleation temperature by certain heating rate, and constant temperature certain hour, so circulation.Initial spontaneous nucleation temperature T
s1it is the most important experiment parameter that carries out SSA research.Usually will in sample, exist the minimum temperature in melting microfacies district as the initial spontaneous nucleation temperature of carrying out SSA research.At this temperature, temperature is enough to most polymer crystallization melting, and simultaneous temperature is enough low can make in sample to exist the fraction crystallization to serve as the nucleus of spontaneous nucleation.[M ü ller, the A.J. such as application M ü ller; Arnal, M.L.Prog.Polym.Sci.2005,30,559-603.] the single step spontaneous nucleation program of report determines the initial spontaneous nucleation temperature of sample.By lot of experiments, show, for this paper for the BOPP PP Pipe Compound, preferably 170～160 ℃ of the initial spontaneous nucleation temperature of detection.After hot classification process completes, adopt the rate of heat addition of 1～20 ° of C/min to record the melting curve of sample.
The method of Fast Evaluation BOPP special materials processing line speed of the present invention, comprise the steps:
(1) based on differential scanning calorimeter, adopt the continuous spontaneous nucleation hot classification technique of annealing to obtain melting curve after hot classification;
(2) quantize to get the I peak of melting peak on curve, start first peak of meter from high temperature, locate for 175 ℃; The II peak, 170 ℃, peak type difference, with the ratio (H of the height of two melting peaks
i/ H
iI) or the ratio (S of area
i/ S
iI) physical quantity σ means;
(3) according to the result of step (2), but the manufacturing limit linear velocity of carrying out the BOPP PP Pipe Compound is judged: σ≤2, and more than the processing line speed of BOPP PP Pipe Compound reaches 420m/min, can High-speed machining; σ>2, BOPP PP Pipe Compound processing line speed, below 420m/min, belongs to low speed processing PP Pipe Compound; When the σ value is less, processing line speed is higher; The polypropylene used of described BOPP PP Pipe Compound is Noblen and/or propylene and C2, the C4-C12 alkene multipolymer through comonomer.Described C2, C4-C12 olefin comonomer are one or more in ethene, butylene, hexene or octene.Described polyethylene pipe material comprises the pellet that is mixed, compressing tablet material, extruded stock or the finished film material after polypropylene powder, pellet, interpolation several functions auxiliary agent, pigment.The described detection BOPP crystallizable isotactic sequence distribution of PP Pipe Compound (wafer thickness distribution) adopts the hot classification technique based on differential scanning calorimeter, obtains result more accurately.
The present invention distributes and carries out the processing characteristics evaluation of PP Pipe Compound as basis with the crystallizable sequence of BOPP PP Pipe Compound, is characterized in:
(a) polymer molecular structure and condensed state structure are combined, can to solid powder, granulation material and the sheet stock of BOPP resin even form film material structure analyzed.This method not only more approaches the actual use procedure of BOPP, and has contained the stages of its processing.Therefore to this, multi-level structure is tested and is analyzed, to the evaluation of the performance of PP Pipe Compound with control more effective.And the method is from affecting the Fundamentals of material property, raw molecule structure and aggregated structure are associated to resolve to the difference of the processing characteristics of BOPP PP Pipe Compound.
(b) be compared to conventional melt flow rate, isotacticity and Mechanics Performance Testing, the analysis of condensed state structure is deep into to the level of molecular stuffing and motion in solid material, understanding for material microstructure is more deep, therefore the evaluation of performance is had more to accuracy and validity.
(c) this method of testing adopts extensively universal this common existing equipment of differential scanning calorimeter to obtain the chain structure of material, the on-line analysis of even practicable production run, so range of application is more extensive.Thus, but key of the present invention is from the test of solid BOPP chain structure and the evaluation method of development to the processing line speed of BOPP PP Pipe Compound analyzing.Characteristics of the present invention are that the crystallizable sequence length of quantitatively characterizing BOPP (wafer thickness) distributes, but extract this physical quantity of ratio σ of two crystallizable sequence length amounts the highest and accordingly the manufacturing limit linear velocity of BOPP estimated.From the performance of BOPP PP Pipe Compound, if long crystallizable isotactic sequence segment too high levels in PP Pipe Compound can make thick wafer too much in PP Pipe Compound form, in machine-shaping, the melting of these wafer orientation needs more energy, more difficult stretch orientation.This can make PP Pipe Compound in film forming heterogeneity in forming process, easily forms the brilliant generation of putting or causing the rupture of membranes phenomenon.If the crystallizable sequence segment of a small amount of length is arranged in PP Pipe Compound, and the segment distribution is relatively concentrated, can crystalline sequence length mostly be long crystallizable sequence segment, and PP Pipe Compound is at the forming process easy-formation.And because crystallizable sequence segment distribution is more concentrated, be characterized in processing characteristics and for the processing characteristics performance of whole PP Pipe Compound, compare homogeneous, but be not easy the rupture of membranes High-speed machining in moulding.
The accompanying drawing explanation
Means of differential scanning calorimetry heating curve after the hot classification that figure 1 – Fig. 6 is BOPP PP Pipe Compound product in corresponding embodiment 1-6 is processed.
Embodiment
Embodiment 1
A kind of powder of BOPP PP Pipe Compound resin, its molten finger and isotacticity and the highest processing line velocity information are as shown in table 1, and its DSC intensification scanning curve after the technical finesse of continuous annealing spontaneous nucleation is as shown in Figure 1.Ratio (the H of the I peak of melting peak on curve (start first peak of meter from high temperature, approximately locate for 175 ℃) II peak (approximately 170 ℃) height
i/ H
iI) or the ratio (S of area
i/ S
iI) physical quantity σ=0.12.The σ of this sample is far smaller than 2, but the manufacturing limit linear velocity of this sample higher than 420m/min, this sample belongs to high speed BOPP PP Pipe Compound.The actual market response situation of evaluation result and sample conforms to.
The sample message of table 1 sample 1
| Test item | MFR，g/10min | Isotacticity, % | The highest processing line speed, m/min |
| Sample 1 | 2.9 | 96.6 | 460 |
Embodiment 2
A kind of pellet of BOPP PP Pipe Compound resin, its molten finger and isotacticity and the highest processing line velocity information are as shown in table 2, and its DSC intensification scanning curve after the technical finesse of continuous annealing spontaneous nucleation is as shown in Figure 2.Ratio (the S of the I peak of melting peak on curve (start first peak of meter from high temperature, approximately locate for 175 ℃) II peak (approximately 170 ℃) area
i/ S
iI) physical quantity σ=2.3.The σ of this sample is greater than 2, but the manufacturing limit linear velocity of this sample belongs to low speed BOPP PP Pipe Compound lower than 420m/min.The actual market response situation of evaluation result and sample conforms to.
The sample message of table 2 sample 2
| Test item | MFR，g/10min | Isotacticity, % | The highest processing line speed, m/min |
| Sample 1 | 2.92 | 96.5 | 380 |
[0024]embodiment 3
Coating materials after a kind of machine-shaping of BOPP PP Pipe Compound resin, its molten finger and isotacticity and the highest processing line velocity information are as shown in table 3, and its DSC intensification scanning curve after the technical finesse of continuous annealing spontaneous nucleation is as shown in Figure 3.Ratio (the H of the I peak of melting peak on curve (start first peak of meter from high temperature, approximately locate for 175 ℃) II peak (approximately 170 ℃) height
i/ H
iI) σ=0.45.The σ of this sample is less than 2, but this sample manufacturing limit linear velocity belongs to high speed BOPP PP Pipe Compound lower than 420m/min.The actual market response situation of evaluation result and sample conforms to.
The sample message of table 3 sample 3
| Test item | MFR，g/10min | Isotacticity, % | The highest processing line speed, m/min |
| Sample 1 | 2.9 | 96.7 | 450 |
Embodiment 4
Coating materials after a kind of machine-shaping of BOPP PP Pipe Compound resin, its molten finger and isotacticity and the highest processing line velocity information are as shown in table 4, and its DSC intensification scanning curve after the technical finesse of continuous annealing spontaneous nucleation is as shown in Figure 4.Ratio (H I/H II) σ=2.9 of the I peak of melting peak on curve (start first peak of meter from high temperature, approximately locate for 175 ℃) II peak (approximately 170 ℃) height.The σ of this sample is greater than 2, but this sample manufacturing limit linear velocity belongs to low speed BOPP PP Pipe Compound lower than 420m/min.The actual market response situation of evaluation result and sample conforms to.
The sample message of table 4 sample 4
| Test item | MFR，10min | Isotacticity, % | The highest processing line speed, m/min |
| Sample 1 | 3.0 | 96.4 | 280 |
Embodiment 5
A kind of pellet of BOPP PP Pipe Compound resin, its molten finger and isotacticity and the highest processing line velocity information are as shown in table 5, and its DSC intensification scanning curve after the technical finesse of continuous annealing spontaneous nucleation is as shown in Figure 5.Ratio (the H of the I peak of melting peak on curve (start first peak of meter from high temperature, approximately locate for 175 ℃) II peak (approximately 170 ℃) height
i/ H
iI) σ=0.The σ of this sample is less than 2, and the accessible limit process velocity of this sample is higher, but the manufacturing limit linear velocity belongs to high speed BOPP PP Pipe Compound higher than 420m/min.The actual market response situation of evaluation result and sample conforms to.
The sample message of table 5 sample 5
| Test item | MFR，g/10min | Isotacticity, % | The highest processing line speed, m/min |
| Sample 1 | 3.1 | 95.1 | 500 |
Embodiment 6
A kind of pellet of BOPP PP Pipe Compound resin, its molten finger and isotacticity and the highest processing line velocity information are as shown in table 6, and its DSC intensification scanning curve after the technical finesse of continuous annealing spontaneous nucleation is as shown in Figure 6.Ratio (the H of the I peak of melting peak on curve (start first peak of meter from high temperature, approximately locate for 175 ℃) II peak (approximately 170 ℃) height
i/ H
iI) σ=1.5.The σ of this sample is less than 2, and the accessible limit process velocity of this sample is taller and bigger in 400m/min, belongs to high speed BOPP PP Pipe Compound.The actual market response situation of evaluation result and sample conforms to.
The sample message of table 6 sample 6
| Test item | MFR，g/10min | Isotacticity, % | The highest processing line speed, m/min |
| Sample 1 | 2.95 | 94.9 | 410 |
Claims (3)
1. the method for a Fast Evaluation BOPP special materials processing line speed is characterized in that:
(1) apply the continuous spontaneous nucleation hot stage division of annealing carries out continuous spontaneous nucleation program test sample and obtains differential scanning calorimetric curve on differential scanning calorimeter;
(2) read from differential scanning calorimetric curve the I peak that quantizes to get melting peak on curve, start first peak of meter from high temperature, locate for 175 ℃; The II peak, 170 ℃; Peak height or calculate two corresponding integral areas of melting peak, obtain the ratio (H of the height of two melting peaks
i/ H
iI) or the ratio (S of area
i/ S
iI);
(3), according to the result of step (2), the manufacturing limit linear velocity of carrying out the BOPP PP Pipe Compound is judged: the ratio of peak height or ratio≤2 of peak area, and more than the processing line speed of BOPP PP Pipe Compound reaches 420m/min, can High-speed machining; If the ratio of peak height or ratio>2 of peak area, BOPP PP Pipe Compound processing line speed, below 420m/min, should be processed under relatively low process velocity.
2. method according to claim 1 is characterized in that: the polypropylene used of described BOPP PP Pipe Compound is Noblen and/or propylene and C2, the C4-C12 alkene multipolymer through comonomer; Described C2, C4-C12 comonomer are one or more in ethene, butylene, hexene, octene or decene multipolymer.
3. method according to claim 1, it is characterized in that: described BOPP PP Pipe Compound comprises polypropylene powder, pellet, compressing tablet material, extruded stock or film article.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106596624A (en) * | 2016-12-21 | 2017-04-26 | 深圳市星源材质科技股份有限公司 | Fractional crystallization analysis method of polyolefin resin |
| CN111024749A (en) * | 2019-12-31 | 2020-04-17 | 常州欣战江特种纤维有限公司 | Method for evaluating spinning post-processing performance based on differential scanning calorimetry |
| CN115232239A (en) * | 2021-04-22 | 2022-10-25 | 中国石油化工股份有限公司 | Ethylene-butene-octene terpolymer and preparation method and system thereof |
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| KR20010084132A (en) * | 2000-02-24 | 2001-09-06 | 유현식 | Method for measuring tactic unit distribution in homo polypropylene using thermal fractionated crystallization and differential scanning calorimetry analysis |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106596624A (en) * | 2016-12-21 | 2017-04-26 | 深圳市星源材质科技股份有限公司 | Fractional crystallization analysis method of polyolefin resin |
| CN111024749A (en) * | 2019-12-31 | 2020-04-17 | 常州欣战江特种纤维有限公司 | Method for evaluating spinning post-processing performance based on differential scanning calorimetry |
| CN115232239A (en) * | 2021-04-22 | 2022-10-25 | 中国石油化工股份有限公司 | Ethylene-butene-octene terpolymer and preparation method and system thereof |
| CN115232239B (en) * | 2021-04-22 | 2024-01-19 | 中国石油化工股份有限公司 | Ethylene-butene-octene terpolymer and preparation method and system thereof |
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Application publication date: 20131218 |