CN105548061A - Identification of polymers and dispersants in rubber adhesive R80 - Google Patents
Identification of polymers and dispersants in rubber adhesive R80 Download PDFInfo
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- CN105548061A CN105548061A CN201510908709.6A CN201510908709A CN105548061A CN 105548061 A CN105548061 A CN 105548061A CN 201510908709 A CN201510908709 A CN 201510908709A CN 105548061 A CN105548061 A CN 105548061A
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- polymkeric substance
- master batch
- infrared
- spreading agent
- rubber
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- 229920001971 elastomer Polymers 0.000 title claims abstract description 24
- 239000005060 rubber Substances 0.000 title claims abstract description 24
- 229920000642 polymer Polymers 0.000 title claims abstract description 10
- 239000000853 adhesive Substances 0.000 title abstract description 9
- 230000001070 adhesive effect Effects 0.000 title abstract description 9
- 239000002270 dispersing agent Substances 0.000 title abstract 4
- 238000012360 testing method Methods 0.000 claims abstract description 52
- 238000000034 method Methods 0.000 claims abstract description 50
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 37
- 238000002137 ultrasound extraction Methods 0.000 claims abstract description 20
- 239000012153 distilled water Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000000862 absorption spectrum Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims abstract description 7
- 239000007864 aqueous solution Substances 0.000 claims abstract description 3
- 238000004566 IR spectroscopy Methods 0.000 claims abstract 3
- 239000000126 substance Substances 0.000 claims description 49
- 239000003292 glue Substances 0.000 claims description 33
- 239000003795 chemical substances by application Substances 0.000 claims description 32
- 238000003892 spreading Methods 0.000 claims description 32
- 230000007480 spreading Effects 0.000 claims description 32
- 239000002904 solvent Substances 0.000 claims description 23
- 238000000576 coating method Methods 0.000 claims description 13
- 239000013078 crystal Substances 0.000 claims description 13
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 12
- 239000007767 bonding agent Substances 0.000 claims description 12
- 238000004090 dissolution Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 8
- -1 methenyl choloride Chemical compound 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 238000009423 ventilation Methods 0.000 claims description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- 239000004215 Carbon black (E152) Substances 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 150000008282 halocarbons Chemical class 0.000 claims description 4
- 229930195733 hydrocarbon Natural products 0.000 claims description 4
- 150000002430 hydrocarbons Chemical class 0.000 claims description 4
- 239000004570 mortar (masonry) Substances 0.000 claims description 4
- 238000012797 qualification Methods 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 3
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 claims description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 3
- 150000002576 ketones Chemical class 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims 1
- 238000001914 filtration Methods 0.000 abstract 1
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 16
- 238000010521 absorption reaction Methods 0.000 description 14
- 239000000463 material Substances 0.000 description 8
- 235000014113 dietary fatty acids Nutrition 0.000 description 7
- 239000000194 fatty acid Substances 0.000 description 7
- 229930195729 fatty acid Natural products 0.000 description 7
- 238000002329 infrared spectrum Methods 0.000 description 7
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 7
- 238000005452 bending Methods 0.000 description 6
- 150000004665 fatty acids Chemical class 0.000 description 5
- 239000005038 ethylene vinyl acetate Substances 0.000 description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 4
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229920003048 styrene butadiene rubber Polymers 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical group [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- CSJDCSCTVDEHRN-UHFFFAOYSA-N methane;molecular oxygen Chemical compound C.O=O CSJDCSCTVDEHRN-UHFFFAOYSA-N 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000004513 sizing Methods 0.000 description 2
- 239000000344 soap Substances 0.000 description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- HIMXAERGQMNODV-UHFFFAOYSA-N 2-N,4-N,1,2,3,4-hexamethoxy-2-N-methyl-1,3,5-triazine-2,4,6-triamine Chemical compound CONC1(N(C(N(C(=N1)N)OC)(N(C)OC)OC)OC)OC HIMXAERGQMNODV-UHFFFAOYSA-N 0.000 description 1
- RHAXKFFKGZJUOE-UHFFFAOYSA-N 7-acetyl-6-ethyl-3,5,8-trihydroxy-9,10-dioxoanthracene-1,2-dicarboxylic acid Chemical compound O=C1C2=CC(O)=C(C(O)=O)C(C(O)=O)=C2C(=O)C2=C1C(O)=C(CC)C(C(C)=O)=C2O RHAXKFFKGZJUOE-UHFFFAOYSA-N 0.000 description 1
- 229920002943 EPDM rubber Polymers 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 244000043261 Hevea brasiliensis Species 0.000 description 1
- 229920000459 Nitrile rubber Polymers 0.000 description 1
- 239000005062 Polybutadiene Substances 0.000 description 1
- 238000012356 Product development Methods 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- HUFIRBOBXZUFPV-UHFFFAOYSA-N benzene-1,3-diol Chemical compound OC1=CC=CC(O)=C1.OC1=CC=CC(O)=C1 HUFIRBOBXZUFPV-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 210000000481 breast Anatomy 0.000 description 1
- 229920005549 butyl rubber Polymers 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- LRCFXGAMWKDGLA-UHFFFAOYSA-N dioxosilane;hydrate Chemical compound O.O=[Si]=O LRCFXGAMWKDGLA-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 229920005555 halobutyl Polymers 0.000 description 1
- 235000010299 hexamethylene tetramine Nutrition 0.000 description 1
- 239000004312 hexamethylene tetramine Substances 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 238000009533 lab test Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229960004011 methenamine Drugs 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229920003052 natural elastomer Polymers 0.000 description 1
- 229920001194 natural rubber Polymers 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920002857 polybutadiene Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000010734 process oil Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000010057 rubber processing Methods 0.000 description 1
- 229960004029 silicic acid Drugs 0.000 description 1
- 229960001866 silicon dioxide Drugs 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 230000005619 thermoelectricity Effects 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
Landscapes
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention provides a method for identifying polymers and dispersants in a rubber adhesive R80 through infrared spectroscopy. The method comprises the following steps: 1) preparing a particle sample from R80 master batch, carrying out ultrasonic extraction with distilled water, carrying out filtering to remove an aqueous solution and repeating the above-mentioned operations 3 to 10 times; 2) placing the sample having undergone ultrasonic extraction in a baking oven for drying; and 3) testing the dried master batch adhesive by using infrared spectroscopy and identifying the types of the polymers and dispersants in the rubber adhesive R80 through the infrared characteristic absorption spectrum of the master batch adhesive. The invention provides a plurality of infrared spectroscopic testing methods for the polymers and dispersants; and the methods are diversified, flexible and optional and can meet needs of testing in laboratories of different configuration levels.
Description
Technical field
The invention belongs to rubber industry field, be specifically related to rubber be carrier rubber adhesive R80 in the qualification of polymkeric substance and spreading agent.
Background technology
In rubber industry, bonding refers to that rubber contacts with homogeneity or dissimilar materials surface, by the combination that the physical action of Van der Waals force or the chemical action of bonding force produce.Usually, the material that material adjacently situated surfaces integrally combines being called bonding agent.In the rubber processing such as tire, conveying belt, sebific duct, the chemical substance of reactivity will be had with addition of one or more, can be there is the chemical bonding of rubber and fabric or steel-wire carcass material in this material, this kind of chemical substance is exactly bonding type bonding agent under curing temperature.Resorcinol-formaldehyde-silica adhesion system is the main binder kind used in rubber industry manufacture both at home and abroad at present, by resorcinol (resorcinol) donor, methylene donor (hexamethoxy methyl cyanuramide HMMM or hexamethylene tetramine HMT) and white carbon (hydrated silicon dioxide, Hydratedsilica) three part compositions, can directly add in sizing material, be called HRH binding system in the world.
R80 is the one of resorcinol donor, and it is the compound of 80% resorcinol and 20% polymkeric substance, is the kneading of resorcinol, spreading agent and polymkeric substance, granulation to be formed in a heated condition.Be pre-dispersed in by resorcinol in polymer support, not only increase the dispersiveness of resorcinol in sizing material, and reduce the irritating smog in mixing action, operability, the feature of environmental protection and security are higher.Current R80 product is on the market a lot, and manufacturer is different, and the polymkeric substance of use is different with the kind of spreading agent.Conventional polymkeric substance has one in natural rubber, butadiene rubber, styrene-butadiene rubber, butyl rubber, halogenated butyl rubber, ethylene-propylene-diene rubber, nitrile rubber, EVA, polyurethane or its compound, and conventional spreading agent has wax, process oil, silicone oil, inorganic filler, fatty acid, derivative of fatty acid etc.
The present invention aims to provide the authentication method of polymkeric substance and fatty acid spreading agent in a kind of R80, with the compositional difference helping rubber industry personnel to contrast various R80 adhesive product on market, for the raw material of tire plant contrast, product purchasing etc. provides foundation.Simultaneously also provide method support, for each product development of rubber industry provides Informational support and foundation for insider understands the technique change that domestic and international producer R80 produces in time.
Summary of the invention
The invention provides one and utilize infrared spectrum, in conjunction with a series of pre-treatment means, measure the analytical approach of polymkeric substance and spreading agent in rubber adhesive R80.
Realizing technical scheme of the present invention is:
The rubber authentication method of polymkeric substance and spreading agent in bonding agent R80, comprises the following steps:
1, R80 master batch is made 2mm
3-5mm
3particle, get 1 weight portion particulate samples in vial, add 50 ~ 10000 weight portion distilled water ultrasonic extraction 10 ~ 60min, filter and discard aqueous solution, repeat aforesaid operations 3 ~ 10 times;
2, the sample after ultrasonic extraction is placed in baking oven to dry, obtains dry master batch glue;
3, with the dried master batch glue of examination of infrared spectrum, by the type of polymkeric substance and spreading agent in the infrared signature absorption spectrum qualification R80 of master batch glue.
Wherein, the optional method of infrared analysis has one or more in KBr pressed disc method, coating method, infrared attenuation full reflection (ATR) method, preferred ATR method.
Wherein KBr pressed disc method gets dry master batch glue to be mixed evenly in agate mortar with dry KBr, fully after grinding, between backform potpourri being put into equably solid preform mould and bed die, then mould put into pressing machine, at 4-12T/cm
2, preferred 8T/cm
2keep within 1-2 minute, obtaining transparent or even translucent ingot sheet under the pressure of left and right.Take out ingot sheet, load in solid sample testing jig, infrared spectrometer is tested.
Wherein coating method is after the master batch glue dissolution with solvents by drying, is applied in getting appropriate dissolution homogeneity on KBr salt sheet, is placed in infrared lamp or ventilation by after clean for solvent volatilization, tests with infrared spectrometer.Can be wherein one or more in hydrocarbon, halogenated hydrocarbons for dissolving the solvent of master batch glue, one or more in preferred methylene chloride, methenyl choloride, toluene, tetrahydrofuran.
Wherein ATR method is directly tested under master batch glue is directly placed in ATR annex, and the crystal wafer of use is selected from Ge crystal wafer or ZnSe crystal wafer.
If in master batch glue spreading agent or polymkeric substance infra-red absorbance signals faint or influence each other, distinguish difficulty, then continuation following steps are tested:
4, the master batch glue of described drying is placed in vial, solubilizer ultrasonic extraction 10 ~ 30min; The solvent wherein chosen is one or more in alcohol, ketone, preferred alcohol, acetone;
5, extract is separated with the polymkeric substance after extraction, tests infrared spectrum respectively, obtain the test result of spreading agent and polymkeric substance;
Wherein, the test of extract, extract test has two kinds of methods: method one (KBr pressed disc method), extract is dried, add dry KBr to be mixed evenly in agate mortar, fully after grinding, sheeter is made transparent or even translucent ingot sheet, load in solid sample testing jig, infrared spectrometer is tested; Method two (coating method), is applied in extract Direct Uniform on KBr salt sheet, is placed in infrared lamp or ventilation by after clean for solvent volatilization, tests with infrared spectrometer.
The test of polymkeric substance, polymkeric substance test has two kinds of methods: method one (coating method), after being dried by polymkeric substance, dissolution with solvents, be applied in getting appropriate dissolution homogeneity on KBr salt sheet, be placed in infrared lamp or ventilation by after clean for solvent volatilization, test with infrared spectrometer; Can be wherein one or more in hydrocarbon, halogenated hydrocarbons for the solvent of dissolve polymer, one or more in preferred methylene chloride, methenyl choloride, toluene, tetrahydrofuran; Method two (ATR method), after being dried by polymkeric substance, directly test under being directly placed in ATR annex, the crystal wafer of use is selected from Ge crystal wafer or ZnSe crystal wafer.
Beneficial effect of the present invention is:
(1) utilize resorcinol water-soluble, spreading agent and polymkeric substance indissoluble or water-fast feature, by aqueous solvent, resorcinol is extracted rejecting from master batch glue, the infrared absorption of spreading agent and polymkeric substance is not disturbed by resorcinol, high-visible, make by the method for the qualitative spreading agent of infrared spectrum and polymkeric substance feasible.
(2) provide multiple infrared spectrum to the method for testing of spreading agent and polymkeric substance, method is various, flexible and selectable, needed for the laboratory test that can meet different configuration level.
Accompanying drawing explanation
R80 infrared absorption spectra in Fig. 1 embodiment 1.
The infrared absorption spectra of R80 master batch glue ATR method test in Fig. 2 embodiment 1.
The infrared absorption spectra of R80 master batch glue ATR method test in Fig. 3 embodiment 2.
The infrared absorption spectra of R80 spreading agent coating method test in Fig. 4 embodiment 2.
The infrared absorption spectra of R80 polymer coating film method test in Fig. 5 embodiment 2.
The infrared absorption spectra of R80 master batch glue coating method test in Fig. 6 embodiment 3.
The infrared absorption spectra of R80 master batch glue ATR method test in Fig. 7 embodiment 4.
Embodiment
Embodiment 1: get 500mg R80 product, cut as 4mm with scissors
3the particle of left and right, by particulate samples in vial, adds 50g distilled water ultrasonic extraction 1h, outwells extract, continue to add distilled water ultrasonic extraction 1h, repeats this step 3 time; Sample is placed in baking oven dry; Take out dry master batch glue and be placed in infrared spectrometer, use the ATR annex test of Ge crystal wafer.
Detecting information is as follows:
Instrument: Nicolet6700 intelligence Fourier infrared spectrograph, thermoelectricity (Shanghai) tech equipment company limited.
Condition: wave-number range: 4000cm
-1~ 600cm
-1; Resolution 4cm
-1, data point interval 1.928cm
-1, scan 32 times.
Test result is shown in accompanying drawing 2.
Conclusion: as shown in Figure 2,966.3cm
-1place is the C-H out-of-plane bending vibration of trans Isosorbide-5-Nitrae C=CH in styrene-butadiene rubber, 911.2cm
-1place is deformation vibration outside vinyl (poly-1,2 structures) face, 759.5cm
-1, 699.0cm
-1two places are the monosubstituted C-H out-of-plane bending vibration of phenyl ring, and spectrogram illustrates that the component of polymer that R80 adopts is the poly-butadiene-styrene rubber of breast; And 1705.2cm
-1, 1736.5cm
-1two places are the characteristic peak of carboxylic carbonyl and ester carbonyl group respectively, 717.7cm
-1place is characteristic peak during long-chain compound methylene chain (n>=4), so the composition of spreading agent that R80 adopts is fatty acid and fatty acid ester.
Embodiment 2: get about 100mg R80 product, cut as 5mm with scissors
3the particle of left and right, by particulate samples in vial, adds 30g distilled water ultrasonic extraction 1h, outwells extract, continue to add distilled water ultrasonic extraction 1h, repeats this step 3 time; Sample is moved on surface plate, be placed in baking oven and dry.Take out dry master batch glue and be placed in infrared spectrometer, use the test of ATR annex Ge crystal wafer.Testing tool and condition are with embodiment 1, and test result is shown in accompanying drawing 3.
(1737.3cm is absorbed apart from obvious ester group as shown in Figure 3 in sample
-1) outward, other absorption peak is feature all not, cannot go out the type of polymkeric substance and spreading agent by precise Identification, need continue experiment, experimental implementation is as follows:
The master batch glue of drying is placed in vial, adds 10mL absolute ethyl alcohol ultrasonic extraction 15min; A small amount of extract uniform application is pipetted on KBr salt sheet with glass capillary; Solvent volatilization is baked to clean, with the test of Nicolet6700 intelligence Fourier infrared spectrograph under the salt sheet smearing extract is placed in infrared lamp.Test condition is: resolution 4cm
-1, data point interval 1.928cm
-1, scan 32 times, blank salt sheet is background.Test result is shown in accompanying drawing 4.
Alcohol extraction liquid in vial is discarded, continues to add 10mL absolute ethyl alcohol ultrasonic extraction 15min, after operating twice more than repeating, sample is moved on surface plate, be placed in baking oven and dry; Take out dried polymkeric substance, dissolve with methenyl choloride, be applied in getting appropriate dissolution homogeneity on KBr salt sheet, be baked to solvent volatilization under being placed in infrared lamp clean, with the test of Nicolet6700 intelligence Fourier infrared spectrograph.Test condition is: resolution 4cm
-1, data point interval 1.928cm
-1, scan 32 times, blank salt sheet is background.Test result is shown in accompanying drawing 5.
Conclusion: from the infrared spectrum (Fig. 4) of extract, except C-H characteristic absorption (2917.3cm
-1, 2849.9cm
-1the asymmetric of methylene and symmetrical stretching vibration absorption peak respectively; 1457.5cm
-1c-CH
3asymmetric bending vibration absorption peak and-CH
2-flexural vibrations absorption peak, 721.4cm
-1for-(CH
2)
n-rocking vibration absorbs), also have the characteristic absorption (1737.7cm of strong ester carbonyl group outward
-1) and carbon oxygen singly-bound stretching vibration absorption (1244.1 ~ 1179.3cm
-1), therefore spreading agent is fatty acid ester material.
From the infrared spectrum (Fig. 5) of polymkeric substance, 2922.5cm
-1, 2852.0cm
-1two places are the asymmetric of methylene and symmetrical stretching vibration, 1464.4cm
-1the flexural vibrations of methylene and the asymmetric curvature vibration of methyl, 1376.4cm
-1the deformation vibration of methyl, 720.8cm
-1for the rocking vibration of methylene, this illustrates that this R80 sample polymkeric substance used is ethylene-propylene diene copolymer (EPDM).
Embodiment 3: get about 100mg R80 product, cut as 4mm with scissors
3the particle of left and right, by particulate samples in vial, adds 20ml distilled water ultrasonic extraction 1h, outwells extract, continue to add distilled water ultrasonic extraction 1h, repeats this step 3 time; Sample is placed in baking oven dry; Take out dry master batch glue and be placed in infrared spectrometer, use the ATR annex test of Ge crystal wafer.Testing tool and conditions see example 1.Test result is shown in accompanying drawing 6.
Conclusion: as shown in Figure 6,1735.4cm
-1the characteristic peak of ester carbonyl group, 1639.0cm
-1the stretching vibration of unsaturated C=C key, 1451.6cm
-1c-CH
3asymmetric bending vibration absorption peak and-CH
2-flexural vibrations absorption peak, 1370.8cm
-1the flexural vibrations of methyl, 1240.4cm
-1for the stretching vibration of C-O in O-C=O, 1161.5cm
-1~ 1034.1cm
-1for carbon oxygen singly-bound stretching vibration absorption peak, 719.3cm
-1for fatty acid-(CH
2) n-rocking vibration absorption peak, above infrared signature peak illustrates in seed lac containing EVA (ethylene-vinyl acetate copolymer).
966.2cm-1 is in styrene-butadiene rubber trans 1, the C-H out-of-plane bending vibration of 4-C=CH, 909.2cm-1 is deformation vibration outside vinyl (poly-1,2 structures) face, 759.2cm-1,699.8cm-1 are the monosubstituted C-H out-of-plane bending vibration of phenyl ring, and spectrogram illustrates in master batch glue containing butadiene-styrene rubber.
To sum up, the polymkeric substance that uses of known this R80 sample compound that is EVA and butadiene-styrene rubber.
Embodiment 4: get certain R80 product and be about 150mg, cut as 4mm with scissors
3the particle of left and right, by particulate samples in vial, adds 30g distilled water ultrasonic extraction 1h, outwells extract, continue to add distilled water ultrasonic extraction 1h, repeats this step 3 time; Sample is placed in baking oven dry; Take out dry master batch glue and be placed in infrared spectrometer, use the ATR annex test of Ge crystal wafer.Testing tool and condition details are with embodiment 1.Test result is shown in accompanying drawing 7.
Conclusion: as shown in Figure 7,2922.6cm
-1, 2851.5cm
-1the asymmetric of methylene and symmetrical stretching vibration, 1399.7cm
-1the deformation vibration of methyl, 722.5cm
-1for the rocking vibration of methylene, this illustrates that this R80 sample polymkeric substance used is EPDM glue; 1548.7cm
-1for the characteristic absorption peak of C=O key in fatty acid soaps salt, illustrate in this sample that adding soap is equally spreading agent.1456.2cm
-1, 872.4cm
-1absorption also illustrate in this sample containing the composition of calcium carbonate.
Claims (9)
1. the rubber authentication method of polymkeric substance and spreading agent in bonding agent R80, is characterized in that, comprise the following steps:
(1) R80 master batch is made 2mm
3-5mm
3particle, get 1 weight portion particulate samples in vial, add 50 ~ 10000 weight portion distilled water ultrasonic extraction 10 ~ 60min, filter and discard aqueous solution, repeat aforesaid operations 3 ~ 10 times;
(2) sample after ultrasonic extraction is placed in baking oven to dry, obtains dry master batch glue;
(3) dried master batch glue is tested with infrared spectrometer, by the type of polymkeric substance and spreading agent in the infrared signature absorption spectrum qualification R80 of master batch glue.
2. the authentication method of polymkeric substance and spreading agent in rubber bonding agent R80 according to claim 1, it is characterized in that, infrared test is selected from one or more in KBr pressed disc method, coating method, infrared attenuation full reflection (ATR) method, preferred ATR method;
Wherein KBr pressed disc method gets dry master batch glue to be mixed evenly in agate mortar with dry KBr, fully after grinding, between backform potpourri being put into equably solid preform mould and bed die, then mould put into pressing machine, at 4-12T/cm
2pressure under keep 1-2 minute, obtain transparent or even translucent ingot sheet, take out ingot sheet, load in solid sample testing jig, infrared spectrometer is tested;
Wherein coating method obtains solution after master batch glue dissolution with solvents by drying, is applied on KBr salt sheet with getting appropriate described dissolution homogeneity, is placed in infrared lamp or dry ventilation by after clean for solvent volatilization, tests with infrared spectrometer;
Wherein ATR method is directly tested with infrared spectrometer under the master batch glue of drying is directly placed in ATR annex; The crystal wafer wherein used is selected from Ge crystal wafer or ZnSe crystal wafer.
3. the authentication method of polymkeric substance and spreading agent in rubber bonding agent R80 according to claim 2, is characterized in that, is one or more in hydrocarbon, halogenated hydrocarbons in coating method for dissolving the solvent of master batch glue.
4. the authentication method of polymkeric substance and spreading agent in bonding agent R80 of the rubber according to any one of claim 2 ~ 3, it is characterized in that, be one or more in methylene chloride, methenyl choloride, toluene, THF for dissolving the solvent of master batch glue in coating method.
5. the authentication method of polymkeric substance and spreading agent in rubber bonding agent R80 according to claim 1, it is characterized in that, if the infrared spectroscopy signals of spreading agent or polymkeric substance is faint or influence each other in described master batch glue, distinguish difficulty, then continuation following steps are tested:
(4) the master batch glue of described drying is placed in vial, solubilizer ultrasonic extraction 10-30min;
(5) extract is separated with the polymkeric substance after extraction, tests with infrared spectrometer respectively, obtain the infrared test result of spreading agent and polymkeric substance;
Wherein, extract test is selected from following two kinds of methods: method one KBr pressed disc method, extract is dried, add dry KBr to be mixed evenly in agate mortar, after abundant grinding, sheeter is made transparent or even translucent ingot sheet, loads in solid sample testing jig, infrared spectrometer is tested; Method two coating method, is applied in extract Direct Uniform on KBr salt sheet, is placed in infrared lamp or dry ventilation by after clean for solvent volatilization, tests with infrared spectrometer;
Polymkeric substance test is selected from following two kinds of methods: method one coating method, and after being dried by polymkeric substance, dissolution with solvents, is applied on KBr salt sheet with getting appropriate dissolution homogeneity, is placed in infrared lamp or ventilation by after clean for solvent volatilization, tests with infrared spectrometer; Method two ATR method, after being dried by polymkeric substance, directly tests with infrared spectrometer under being directly placed in ATR annex.
6. the authentication method of polymkeric substance and spreading agent in rubber bonding agent R80 according to claim 5, is characterized in that, in step (4) during ultrasonic extraction master batch glue, the solvent chosen is one or more in alcohol, ketone.
7. the authentication method of polymkeric substance and spreading agent in rubber bonding agent R80 according to claim 6, is characterized in that, in step (4) during ultrasonic extraction master batch glue, the solvent chosen is at least one in ethanol, acetone.
8. the authentication method of polymkeric substance and spreading agent in rubber bonding agent R80 according to claim 5, is characterized in that, in the test of polymkeric substance, the solvent of dissolve polymer is one or more in hydrocarbon, halogenated hydrocarbons.
9. the authentication method of polymkeric substance and spreading agent in rubber bonding agent R80 according to claim 8, it is characterized in that, in the test of polymkeric substance, the solvent of dissolve polymer is at least one in methylene chloride, methenyl choloride, toluene, tetrahydrofuran.
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