CN1432802A - Fast infrared spectrometric process of isotactic degree of biaxial stretched polypropylene - Google Patents
Fast infrared spectrometric process of isotactic degree of biaxial stretched polypropylene Download PDFInfo
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- CN1432802A CN1432802A CN 02112546 CN02112546A CN1432802A CN 1432802 A CN1432802 A CN 1432802A CN 02112546 CN02112546 CN 02112546 CN 02112546 A CN02112546 A CN 02112546A CN 1432802 A CN1432802 A CN 1432802A
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Abstract
The fast infrared spectrometric process of isotactic degree of biaxial stretched polypropylene includes the steps of preparing sample sheets, testing sample sheets and data processing. Two film sample sheets in the same thickness are prepared by heating in mold to 175 deg.c, pressurizing to 4t, maintaining for less than 2 sec, relieving and coooling. During the testing, the two film sample sheets are inserted into the test rack of infrared spectrometer and measured in several points to obtain transmitted infrared spectrum at 998/cm and 1460 /cm; and the transmitted infrared spectrum is converted into absorbency infrared spectrum. During data processing, the measured spectrum numbers of the two film sample sheets are arranged and the isotactic degree Y is calculated based on Y=75.9308R+73.5054, where R=A998/A1460.
Description
One, technical field
The present invention is a kind of assay method to the biaxial stretch-formed polypropylene isotacticity, especially a kind of method with infra-red sepectrometry fast measuring biaxial stretch-formed polypropylene isotacticity.
Two, background technology
Biaxial stretch-formed polypropylene is called for short BOPP.The film of being made by it has good performance, has to grease the wet infiltration of resistance, wear-resisting, when high temperature, still can provide high-tension, have characteristics such as good low-temperature impact strength and toughness, be widely used in the numerous areas such as cigarette film, light film, pearly-lustre film and packaging for foodstuff.In recent years, rapid, the huge market demand of BOPP development, the added value of product height has become the focus that polypropylene is used.
As everyone knows, polypropylene is the superpolymer of typical tacticity.Its character and tacticity have much relations, and particularly isotacticity is more remarkable to the influence of its crystal property, and isotacticity is high more, and crystallinity is also big more.The hardness of material is big, poor toughness.Polyacrylic elastic modulus is to raise with isotacticity.Therefore, polypropylene isotacticity size directly influences the production run of BOPP film forming and the properties of product of film, so one of important parameter that isotacticity is the BOPP PP Pipe Compound to be produced.
The BOPP PP Pipe Compound has the lower characteristics of isotacticity, and the better physical mechanical property is arranged, the intensity height, transparency is good, and smooth surface is in the drawing process, film forming is good, and the disconnected film that is difficult for breaking is so the control of isotacticity is to produce one of BOPP PP Pipe Compound key parameter.
The method for measuring of polypropylene isotacticity is a lot, as x-ray method, densimetry, melting point method, DSC method, infra-red sepectrometry,
13The C-NMR nuclear magnetic resonance method.Measure in the industrial and laboratory polypropylene isotacticity the most frequently used be the boiling n-heptane extraction, but this method test period is long, generally wants 7～8 hours, and x-ray method, melting point method, DSC method all have similar problem.Though the 13C-NMR nuclear magnetic resonance method is the effective method of test isotacticity, because of the expensive complicated operation of instrument, the cycle is long, incompatibility industrialized production device express-analysis requirement equally.Still there are not unified standard and standard at present with FT-IR infra-red sepectrometry test polypropylene isotacticity.
Three, technology contents
1, goal of the invention:
The infra-red sepectrometry Rapid Determination Method that the purpose of this invention is to provide a kind of isotacticity of biaxial stretch-formed polypropylene fast and accurately.
2, technical scheme:
Biaxial stretch-formed polypropylene isotacticity of the present invention through external spectrum method Rapid Determination Method be: a, produce print: the warm table radiator valve is transferred to 175 ± 1 ℃, the material grain or the powder of sample are placed the metal sheeting mould that serves as a contrast aluminium foil, this mould put into heat up and be stabilized in 175 ± 1 ℃ warm table, when treating that temperature rises to 175 ± 1 ℃ once more, at once be forced into 4t, constant temperature and pressure time＜2 second, at once unload and be depressed into zero-pressure, after extracting the metal sheeting mould out and putting into cooling box and be cooled to room temperature, take out the film print, produce two film prints that thickness is identical by above method; The test of b, print: two film prints will suppressing insert on the test bracket of infrared spectrometer, get any several test point respectively on two prints, survey 998cm
-1And 1460cm
-1Transmits infrared spectrum and conversion or absorbance infrared spectrum; C, data processing: with the above absorbance spectrum value of surveying two film prints series arrangement by size, calculate isotacticity Y=75.9308R+73.5054, R=A wherein
998/ A
1460, the identical film print of producing of two thickness, its thickness difference is less than 5 microns; The wave-number range of infrared spectrometer is set in 4000～400cm
-1Carry out background scans.
3, technique effect:
That the present invention sets up is convenient, FT-IR infrared spectroscopic determination BOPP PP Pipe Compound isotacticity fast and accurately, and test only needed to finish in 1 hour, can adapt to the quick trace analysis requirement that the industrialization bigger device is produced the BOPP PP Pipe Compound.The present invention especially is suitable for the ZiegLer-Natta effective catalyst and produces the BOPP PP Pipe Compound.
Four, specific implementation method
Infrared spectrometer adopts U.S. PE company 1760 type fourier transform infrared spectroscopy instrument, and the molding press of producing print adopts the U.S. SPECAC of PE company molding press, and the test environment temperature is 25 ± 3 ℃, test environment humidity R≤60%.
A, produce print:
1, the temperature with the warm table temperature controller is set in 175 ± 1 ℃;
2, when the temperature of warm table is raised to 175 ± 1 ℃, warm table is wanted constant temperature half an hour, can sample preparation;
3, sample pellet (powder) is placed the metal die of lining aluminium foil (being convenient to peeling off of film), put on the warm table and heat, when treating that temperature is raised to 175 ± 1 ℃ once more, at once be forced into 4t (gauge pressure), constant temperature and pressure time＜2 second (constant voltage time＜2 second) are unloaded at once and are depressed into zero (gauge pressure), the extraction metal die is put into cooling box and is cooled to room temperature, takes out the film print;
4, by two film prints of every kind of sample system of 3 steps FT-IR test
The test of b, print:
(1) whether the temperature of checkout environment, humidity meet the requirements, and operate under the constant temperature of stipulating, constant humidity condition;
(2) FT-IR infrared spectrometer start, stablize 30 minutes after, whether inspection apparatus resolution, energy, signal to noise ratio (S/N ratio) reach the given index of producer, carry out the scanning of 0%, 100% transmitance and background noise, enter next step test operation after normal;
(3) the BOPP sample is pressed the same diaphragm of thickness by sample preparation requirement compacting, diaphragm thickness difference≤5um otherwise from new compacting until conforming with thickness requirement.
(4) set FT-IR infrared spectrometer wave-number range 4000～400
-1Unit carries out background scans;
(5) print that suppresses is inserted on the FT-IR sample test support, measure the transmissivity infrared spectrogram.
(6) make two film prints, take up an official post at every and get (arbitrarily getting) 5 surveys 998cm
-1And 1460cm
-1Transmitted infrared light spectrum and convert to the absorbance infrared spectrum with the absorbance of two spectrum totally 10 groups of data insert in the table.
C, data processing:
1, the isotacticity fraction distributes: with 10 groups of 998cm
-1And 1460cm
-1The infrared spectrum absorbance ratio is series arrangement by size;
2, extremely wide district middle rank divides maximum value: fraction at the same level is maximum in 10 groups of fractions distribute is extremely wide district, and getting its maximal value is maximum value;
3, R value: getting extremely wide district middle rank branch maximum value is the R value, will calculate the isotactic value in this value substitution regression formula;
The special circumstances that run into when 4, getting extremely wide district middle rank branch maximum value in the calculating;
(1) the two groups of wide district of consecutive roots level at the same level mark same cases are arranged in 10 groups of fractions distribute, the arithmetic mean of at this moment getting two groups extremely wide adjacent district's middle rank branch maximum value is the R value;
(2), at this moment need be used in and get on two prints at 10 and survey 2～3 groups of 998cm outward again if 10 groups of fractions have at the same level grade of mark same case in extremely wide district more than two groups in distributing
-1And 1460cm
-1The infrared spectrum absorbance ratio adds by big series arrangement, is the R value from newly finding out the big value of the intermediate classification in extremely wide district;
(3) in distributing, 10 groups of fractions have two groups extremely wide districts level at the same level mark identical but be not that at this moment the extremely wide district of two adjacent groups but (lacking one group of fraction) two groups of extremely wide district situations at interval need get on two prints and survey 2～3 groups of 998cm outside 10 again
-1And 1460cm
-1The infrared spectrum absorbance ratio adds series arrangement by size, is the R value from newly finding out extremely wide district middle rank branch maximum value.
Isotacticity: Y=75.9308R+73.5054
R＝A
998/A
1460
γ＝0.9951
Claims (3)
1, a kind of infra-red sepectrometry Rapid Determination Method of biaxial stretch-formed polypropylene isotacticity is characterized in that assay method is:
A, produce print: the warm table radiator valve is transferred to 175 ± 1 ℃, the material grain or the powder of sample are placed the metal sheeting mould that serves as a contrast aluminium foil, this mould put into heat up and be stabilized in 175 ± 1 ℃ warm table, when treating that temperature rises to 175 ± 1 ℃ once more, be forced into 4t at once, constant temperature and pressure time＜2 second, at once unload and be depressed into zero-pressure, after extracting the metal sheeting mould out and putting into cooling box and be cooled to room temperature, take out the film print, produce two film prints that thickness is identical by above method;
The test of b, print: two film prints will suppressing insert on the test bracket of infrared spectrometer, get any several test point respectively on two prints, survey 998cm
-1And 1460cm
-1Transmits infrared spectrum also converts the absorbance infrared spectrum to;
C, data processing: with the above absorbance spectrum value of surveying two film prints series arrangement by size, calculate isotacticity Y=75.9308R+73.5054, R=A wherein
998/ A
1460
2, the infra-red sepectrometry Rapid Determination Method of biaxial stretch-formed polypropylene isotacticity according to claim 1 is characterized in that the identical film print of two thickness produced, and its thickness difference is less than 5 microns.
3, the infra-red sepectrometry Rapid Determination Method of biaxial stretch-formed polypropylene isotacticity according to claim 1 and 2 is characterized in that the wave-number range of infrared spectrometer is set in 4000～400cm
-1Carry out background scans.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021125465A CN1177215C (en) | 2002-01-17 | 2002-01-17 | Fast infrared spectrometric process of isotactic degree of biaxial stretched polypropylene |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021125465A CN1177215C (en) | 2002-01-17 | 2002-01-17 | Fast infrared spectrometric process of isotactic degree of biaxial stretched polypropylene |
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| Publication Number | Publication Date |
|---|---|
| CN1432802A true CN1432802A (en) | 2003-07-30 |
| CN1177215C CN1177215C (en) | 2004-11-24 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB021125465A Expired - Fee Related CN1177215C (en) | 2002-01-17 | 2002-01-17 | Fast infrared spectrometric process of isotactic degree of biaxial stretched polypropylene |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102156147A (en) * | 2011-03-07 | 2011-08-17 | 四川大学 | Method for detecting film forming stability of polypropylene in bidirectional stretching by using thermal analysis method |
| CN102564988A (en) * | 2010-12-23 | 2012-07-11 | 中国石油化工股份有限公司 | Method for measuring unsaturation degree of sticky solid matter by infrared spectrometer and sample support for same |
| CN102564816A (en) * | 2010-12-23 | 2012-07-11 | 中国石油化工股份有限公司 | Sample preparation method of viscous solid matter and one-hole sample preparation mold used by same |
| CN102879247A (en) * | 2012-10-09 | 2013-01-16 | 神华集团有限责任公司 | Method for manufacturing to-be-measured film for infrared analysis and method for measuring Fc, Ec and Et |
| CN104749128A (en) * | 2015-04-27 | 2015-07-01 | 风帆股份有限公司 | Method for determining ageing time of polypropylene plastic by utilizing infrared spectra |
| CN105806798A (en) * | 2016-05-18 | 2016-07-27 | 成都慧成科技有限责任公司 | Method for quickly measuring different isotacticities of polyvinyl alcohol through infrared spectroscopy |
-
2002
- 2002-01-17 CN CNB021125465A patent/CN1177215C/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102564988A (en) * | 2010-12-23 | 2012-07-11 | 中国石油化工股份有限公司 | Method for measuring unsaturation degree of sticky solid matter by infrared spectrometer and sample support for same |
| CN102564816A (en) * | 2010-12-23 | 2012-07-11 | 中国石油化工股份有限公司 | Sample preparation method of viscous solid matter and one-hole sample preparation mold used by same |
| CN102564988B (en) * | 2010-12-23 | 2015-03-25 | 中国石油化工股份有限公司 | Method for measuring unsaturation degree of sticky solid matter by infrared spectrometer and sample support for same |
| CN102156147A (en) * | 2011-03-07 | 2011-08-17 | 四川大学 | Method for detecting film forming stability of polypropylene in bidirectional stretching by using thermal analysis method |
| CN102156147B (en) * | 2011-03-07 | 2012-07-25 | 四川大学 | Method for detecting film forming stability of polypropylene in bidirectional stretching by using thermal analysis method |
| CN102879247A (en) * | 2012-10-09 | 2013-01-16 | 神华集团有限责任公司 | Method for manufacturing to-be-measured film for infrared analysis and method for measuring Fc, Ec and Et |
| CN102879247B (en) * | 2012-10-09 | 2014-10-08 | 神华集团有限责任公司 | Method for manufacturing to-be-measured film for infrared analysis and method for measuring Fc, Ec and Et |
| CN104749128A (en) * | 2015-04-27 | 2015-07-01 | 风帆股份有限公司 | Method for determining ageing time of polypropylene plastic by utilizing infrared spectra |
| CN105806798A (en) * | 2016-05-18 | 2016-07-27 | 成都慧成科技有限责任公司 | Method for quickly measuring different isotacticities of polyvinyl alcohol through infrared spectroscopy |
| CN105806798B (en) * | 2016-05-18 | 2018-10-02 | 成都慧成科技有限责任公司 | A method of utilizing Polyethylene by Infrared Spectrometry alcohol difference isotacticity |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1177215C (en) | 2004-11-24 |
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Owner name: SINOPEC YANGZI PETROCHEMICAL CO. Free format text: FORMER NAME OR ADDRESS: YANGZI PETROCHEMICAL CO., LTD. |
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Address after: No. 777, Dachang District, Jiangsu, Xinhua Road, Nanjing Patentee after: Sinopec Yangzi Petrochemical Company Ltd. Address before: No. 777, Dachang District, Jiangsu, Xinhua Road, Nanjing Patentee before: Yangtze Petrochemical Industry Co., Ltd. |
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