CN105891140A - Method for measuring blending ratio of halogenated butyl rubber and natural rubber in rubber - Google Patents
Method for measuring blending ratio of halogenated butyl rubber and natural rubber in rubber Download PDFInfo
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- CN105891140A CN105891140A CN201610281180.4A CN201610281180A CN105891140A CN 105891140 A CN105891140 A CN 105891140A CN 201610281180 A CN201610281180 A CN 201610281180A CN 105891140 A CN105891140 A CN 105891140A
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- rubber
- halogenated butyl
- butyl rubber
- natural gum
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- 229920005555 halobutyl Polymers 0.000 title claims abstract description 76
- 229920001971 elastomer Polymers 0.000 title claims abstract description 66
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000002156 mixing Methods 0.000 title abstract description 4
- 244000043261 Hevea brasiliensis Species 0.000 title abstract 6
- 229920003052 natural elastomer Polymers 0.000 title abstract 6
- 229920001194 natural rubber Polymers 0.000 title abstract 6
- 238000002835 absorbance Methods 0.000 claims abstract description 23
- 238000004566 IR spectroscopy Methods 0.000 claims abstract description 10
- 229920001206 natural gum Polymers 0.000 claims description 50
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical group CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- 238000003556 assay Methods 0.000 claims description 13
- 239000003292 glue Substances 0.000 claims description 13
- 238000005336 cracking Methods 0.000 claims description 10
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 8
- 239000000284 extract Substances 0.000 claims description 8
- 238000000197 pyrolysis Methods 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000002329 infrared spectrum Methods 0.000 claims description 6
- 239000003153 chemical reaction reagent Substances 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 4
- 238000011481 absorbance measurement Methods 0.000 claims description 4
- 239000006229 carbon black Substances 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 4
- 229910052717 sulfur Inorganic materials 0.000 claims description 4
- 239000011593 sulfur Substances 0.000 claims description 4
- 239000011787 zinc oxide Substances 0.000 claims description 4
- 238000001228 spectrum Methods 0.000 claims description 2
- 238000012360 testing method Methods 0.000 abstract description 15
- 238000001514 detection method Methods 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 229920000642 polymer Polymers 0.000 description 10
- 238000004458 analytical method Methods 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 229920005556 chlorobutyl Polymers 0.000 description 6
- 238000000045 pyrolysis gas chromatography Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000002411 thermogravimetry Methods 0.000 description 4
- 244000144987 brood Species 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical compound CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 description 2
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical group CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 229920005549 butyl rubber Polymers 0.000 description 2
- 238000003776 cleavage reaction Methods 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 125000004968 halobutyl group Chemical group 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000012797 qualification Methods 0.000 description 2
- 230000007017 scission Effects 0.000 description 2
- 238000005987 sulfurization reaction Methods 0.000 description 2
- OWRCNXZUPFZXOS-UHFFFAOYSA-N 1,3-diphenylguanidine Chemical compound C=1C=CC=CC=1NC(=N)NC1=CC=CC=C1 OWRCNXZUPFZXOS-UHFFFAOYSA-N 0.000 description 1
- CBXRMKZFYQISIV-UHFFFAOYSA-N 1-n,1-n,1-n',1-n',2-n,2-n,2-n',2-n'-octamethylethene-1,1,2,2-tetramine Chemical compound CN(C)C(N(C)C)=C(N(C)C)N(C)C CBXRMKZFYQISIV-UHFFFAOYSA-N 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 210000003484 anatomy Anatomy 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 229920005557 bromobutyl Polymers 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000000539 dimer Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000026030 halogenation Effects 0.000 description 1
- 238000005658 halogenation reaction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- XMGQYMWWDOXHJM-UHFFFAOYSA-N limonene Chemical compound CC(=C)C1CCC(C)=CC1 XMGQYMWWDOXHJM-UHFFFAOYSA-N 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 229920001195 polyisoprene Polymers 0.000 description 1
- -1 polysiloxane Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 238000004227 thermal cracking Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000013638 trimer Substances 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
Abstract
The invention relates to a method for measuring the blending ratio of halogenated butyl rubber and natural rubber in rubber. The method comprises the following steps: measuring the absorbance by infrared spectroscopy using at least three samples of the known rubber, calculating the ratio of the peak height of the halogenated butyl rubber to the sum of the peak heights of the natural rubber and the halogenated butyl rubber according to formula I, R ═ HA/(HA+HB) Formula I; drawing a percentage working curve of the halogenated butyl rubber in the sum of the natural rubber and the halogenated butyl rubber according to the obtained R value; and measuring the absorbance of the rubber to be measured containing the halogenated butyl rubber and the natural rubber by using an infrared spectrometer, and substituting the absorbance into a regression curve to obtain the weight percentage of the halogenated butyl rubber in the total of the natural rubber and the halogenated butyl rubber. The invention has the advantages that: first, only 4000cm of test is needed‑1～400cm‑1The absorbance is high, the operation is convenient and simple, and the separation condition is not required to be groped; secondly, the detection instrument, the consumables and the personnel application cost are low, and the method can be popularized in a large range; thirdly, a clear spectrogram can be obtained.
Description
Technical field
The present invention relates to halogenated butyl rubber and natural gum in a kind of rubber and with than assay method.
Background technology
The analysis of rubber components, for the formula, imitated of the unknown rubber sample that appraises the quality of a product, estimates
New product, all can be provided with the information of directive significance.Anatomy rubber mainly uses with the component of rubber
Method be thermogravimetry, such as ISO 9924-1, ISO 9924-2, ISO 9924-3, all use
Thermogravimetry measures vulcanizate and the composition of uncured rubber, ISO9924-3 be for extracting after hydrocarbon
Rubber, halogenated rubber, polysiloxane-based rubber.Same China standard GB/T/T14837 " rubber and
Rubber thermogravimetry measures vulcanizate and the composition of uncured rubber " it is also classified into three parts, be equally
Thermogravimetry is used to analyze the composition of rubber.
And be chemical analysis for the analysis main method of rubber system composition in Rubber & Rubber Products
And instrumental method.Chemical analysis is mainly combustion characteristic test, thermal decomposition product to the qualification of polymer
Spot test etc. on solution colour test, paper；Polymer content is estimated the kind mainly according to rubber
Class selects suitable chemical reagent by filtering after rubber solution, being re-weighed after drying, is calculated polymer
Content.And instrumental method is mainly gas chromatography and the infrared spectrometry of pyrolysis product, employing is split
Gas chromatography analytic process, such as international standard ISO7270 and GB/T 29613, and GB/T29613 is equivalent
Adopt international standards ISO7270, and this standard is divided into two parts GB/T 29613.1 and GB/T 29613.2,
All use pyrolysis gas chromatography analysis method that polymer is identified.Infrared spectrometry such as ISO 4650 He
GB/T 7764, uses cracking or pours into a mould embrane method discriminating rubber, vulcanizate or last goods, but this skill
Art is limited to single glue and some blend rubber.
For the estimation of polymer content in rubber and rubber, chemical analysis is for single polymers
Qualification and cubage relatively accurate, but identify more difficult for shared type of polymer, and to poly-
The evaluated error of each constituent content of compound is bigger；Instrumental method has bigger advantage compared with chemical analysis,
But the mensuration of composition content each to polymer not regulation；Pyrolysis gas chromatography needs to be equipped with cracker
And gas chromatogram, two parts instrument price is expensive, and maintenance cost is high, and operation also has certain difficulty,
The application of rubber producer has certain limitation.
For halogenated butyl rubber and natural gum used time, wherein halogenated butyl rubber is by halogen (mainly bromine
And chlorine) replace hydrogen butadiene isoprene copolymer, when utilizing pyrolysis gas chromatograph detection technique,
Major cleavage products is isobutene., and its dimer, trimer, the tetramer, pentamer etc. mix
Thing, there will be periodic bunch of peak in chromatogram；Wherein natural gum is the polymer of polyisoprene,
The product of major cleavage is isoprene and cinene.When halogenated butyl rubber and natural gum used time, cracking
In gas chromatogram, each characteristic peak can not reach to be kept completely separate, so, measure by pyrolysis gas chromatography
Halogenated butyl rubber is with natural gum and the most difficult with ratio.
Therefore, it is necessary to propose effective technical scheme, solve the problems referred to above.
Summary of the invention
The present invention is directed to above-mentioned the deficiencies in the prior art, it is provided that halobutyl in a kind of easy to operate rubber
Glue and natural gum and with than assay method.
The technical scheme is that
In a kind of rubber halogenated butyl rubber and natural gum and with than assay method, step is as follows:
1) first application at least three contains the known rubber sample of halogenated butyl rubber and natural gum, with red
External spectrum instrument measures known rubber sample absorbance, calculates halogenated butyl rubber peak height value according to Formulas I and accounts for natural
Glue and the ratio of halogenated butyl rubber peak height value summation,
R=HA/(HA+HB) Formulas I
Wherein, HABe wave number be 1250cm-1～1220cm-1Between the peak of halogenated butyl rubber characteristic peak absorbance
High level, HBIt is that natural gum is at 885cm-1～889cm-1The peak height value of characteristic peak absorbance；
2) according to step 1) the R value that obtains, draw natural gum and halogenated butyl rubber shared by halogenated butyl rubber
The percentage duty curve of summation, particularly as follows: with R value as X-axis, with halogenated butyl rubber account for natural gum and
The percentage by weight of halogenated butyl rubber summation is Y-axis, draws regression curve with method of least square
Y=ax2+bx+c；
3) determination of infrared spectroscopy is utilized to contain the rubber absorbance to be measured of halogenated butyl rubber and natural gum,
Substitute into step 2) in the regression curve that draws, obtain halogenated butyl rubber and account for natural gum and halogenated butyl rubber is total
The percentage by weight of sum.
Further, the step of described determination of infrared spectroscopy known rubber sample absorbance includes:
1) extracting: by the B method of GB/T3516-2006, known rubber sample is stripped, and dries
Sample；
2) absorbance measurement: by step 1) in after extracting the sample that obtains, by cracking product after cracking
Thing infrared spectrometer records infrared spectrum in 2.5 μm～15 μ m wavelength range；Pyrolysis product is existed
Measure absorbance on infrared spectrometer, show that wave number is at 885cm-1～889cm-1And 1250cm-1~
1220cm-1Between peak height value.
Further, raw material and the parts by weight thereof of described known rubber sample are: halogenated butyl rubber and sky
So glue parts by weight and be 100 parts, operate oily 10 weight portions, white carbon black 70 weight portion, age resistor 1
Weight portion, sulfur 1 weight portion, zinc oxide 2 weight portion, accelerator 0.6 weight portion.
Further, described halogenated butyl rubber with the percentage by weight of natural gum is: 0:100,20:80,
40:60,50:50,60:40,70:30,80:20 or 100:0.
Further, described extracting, particularly as follows: extraction solvent is acetone, extracts 12h under 75 DEG C of water bath condition
After, change an acetone reagent, again extract 12h under 75 DEG C of water bath condition, put into after sample is taken out
105 DEG C of baking ovens dry to constant weight.
Compared with prior art, the invention have the advantages that: first, only need to test 4000cm-1～400cm-1
Absorbance, easy to operate simply, be not required to grope separation condition；Second, detecting instrument, consumptive material, people
Member's application cost is low, can promote on a large scale；3rd, spectrogram clearly can be obtained.
Detailed description of the invention
In rubber of the present invention halogenated butyl rubber and natural gum and with than assay method, key step bag
Include: sample preparation steps, sample solvent are extracted stage, infrared spectrum and absorbance measurement stage out, painted
Working curve stage of standard sample processed, measure the rubber stage to be measured.Specifically comprise the following steps that
1) sample preparation steps: use the mixing known rubber sample raw material of same formula, it is known that rubber like
Product are at least 3, and the ratio ranges bag of the halogenated butyl rubber included by known rubber sample and natural gum
It is contained in the halogenated butyl rubber of unknown sample and the scope of natural gum.
As one embodiment of the present of invention, raw material and the parts by weight thereof of described known rubber sample are:
Halogenated butyl rubber and natural gum and be 100phr, operation oily 10phr, white carbon black 70phr, age resistor 1phr,
Sulfur 1phr, zinc oxide 2phr, accelerator 0.6phr.Preferably, described halogenated butyl rubber and natural gum
Percentage by weight is: 0:100,20:80,40:60,50:50,60:40,70:30,80:20 or 100:0.
2) sample solvent extracts the stage out: select suitable solvent, by the B method of GB/T3516-2006 to sample
Product are stripped, dry sample, remove residual solvent, and sample is standby.Preferably, described extracting is concrete
For: extraction solvent is acetone, after extracting 12h, changes an acetone reagent under 75 DEG C of water bath condition, then
Extract 12h under secondary 75 DEG C of water bath condition, put in 105 DEG C of baking ovens after sample is taken out and dry to constant weight.
3) infrared spectrum and the absorbance measurement stage: by step 2) in after extracting the sample that obtains,
After cracking, pyrolysis product capillary tube is drawn and be applied on a small quantity on KBr salt sheet, with infrared spectrometer 2.5
Record infrared spectrum in μm～15 μ m wavelength range；Owing to the scan mode of spectrogram is different, treating
Before surveying rubber testing, it should test known rubber sample on same infrared spectrum instrument, repeat above-mentioned
Step analyzes all known rubber samples for drawing curve；Infrared spectrometer measures extinction
Degree, calculates wave number at 885cm-1～889cm-1And 1250cm-1～1220cm-1Between peak height value, and by peak
High level substitutes into Formulas I, calculates halogenated butyl rubber peak height value according to Formulas I and accounts for natural gum and halogenated butyl rubber peak height value
The ratio of summation,
R=HA/(HA+HB) Formulas I
Wherein, HABe wave number be 1250cm-1～1220cm-1Between the peak of halogenated butyl rubber characteristic peak absorbance
High level, HBIt is that natural gum is at 885cm-1～889cm-1The peak height value of characteristic peak absorbance.
As one embodiment of the present of invention, Fourier transformation spectrogrph selected by described infrared spectrometer, splits
The mode of alcohol burner heating is used during solution
4) draw the working curve stage of standard sample: the R value obtained after cracking according to known rubber sample,
Draw natural gum and the percentage duty curve of halogenated butyl rubber summation shared by halogenated butyl rubber.I.e. with halogenation
The percentage ratio R of natural gum shared by the peak height value of butyl rubber and halogenated butyl rubber peak height value summation is X-axis, with halogen
Changing butyl rubber is Y-axis relative to the percentage ratio of two brood lac summations, draws regression curve with method of least square
Y=ax2+ bx+c, this regression curve is the working curve of standard specimen.It is to be appreciated that be used for drawing mark
The form of the known rubber sample of directrix curve is identical with testing sample, is i.e. uncured rubber or is sulfuration
Glue.Raw material type and the proportioning of each known rubber sample are identical, differ only in halogenated butyl rubber with
Natural gum and different with ratio.
5) the rubber stage to be measured is measured: utilize determination of infrared spectroscopy to contain halogenated butyl rubber and natural gum
Rubber absorbance to be measured, substitute into step 4) in the regression curve that draws, obtain halogenated butyl rubber and account for sky
So glue and percentage by weight of halogenated butyl rubber summation.
The present invention only need to utilize infrared spectrometer to test 4000cm-1-400cm-1Absorbance, easy to operate
Simply, on the basis of existing technology (ISO 4650 and GB/T 7764), it is not required to grope again test strip
Part and sample making technology, only need to determine the halogenated butyl rubber of feature and the target peak of natural gum, then determine work
The empirical equation of curve, sets up the working curve that dependency is good, so that it may measure halogenated butyl rubber with natural
Glue and with ratio, accuracy is high, swift to operate simply.
Test example 1
In in a kind of rubber chlorinated butyl rubber and natural gum and with than assay method, step is as follows:
1) prepared by sample: mixing and cured samples, and sample amounts to 8, and the formula of sample is chlorinated butyl
Glue is 100phr, TDAE oil 10phr with total number of natural gum, and white carbon black N660 is 70phr, age resistor
RD1phr, sulfur 1phr, zinc oxide 2phr, diphenylguanidine is 0.6phr.In 8 samples chlorinated butyl rubber with
The mass percent of natural gum be respectively as follows: 0:100,20:80,40:60,50:50,60:40,70:30,
80:20,100:0, other materials is identical.It is standby that whole white silk glue obtains test piece after sulfuration；
2) sample after vulcanizing 8 is cut into little slice respectively, weighs 1.0g, is put in Soxhlet extractor,
Extracting according to GB/T3516-2006 method B, extraction solvent is acetone, extracts 12h under 75 DEG C of water bath condition
After, change an acetone reagent.Again extract 12h, put in 105 DEG C of baking ovens after sample is taken out and be dried to
Constant weight.
3) thermal cracking: sample is cut into little granule and is put in test tube, cracks under alcohol burner, uses glass
Capillary tube draws pyrolysis product.Pyrolysis product is measured on infrared spectrometer absorbance, calculates wave number and exist
889cm-1And 1230cm-1Peak height value；And peak value is updated to computing formula R=HA/(HA+HBIn), obtain R
Value；
4) drawing curve, with natural gum shared by the peak height value of halogenated butyl rubber and halogenated butyl rubber peak
The percentage ratio R of high level summation is X-axis, with halogenated butyl rubber relative to the percentage ratio of two brood lac summations as Y-axis,
Regression curve y=-332x is drawn with method of least square2+ 372x, this regression curve is the work of 8 standard specimens
Curve.In equation y value represent chlorinated butyl rubber brood lac two in mass percent, x value is halobutyl
The percentage ratio i.e. R value of natural gum shared by the peak height value of glue and halogenated butyl rubber peak height value summation.
5) the rubber stage to be measured is measured: utilize determination of infrared spectroscopy to contain halogenated butyl rubber and natural gum
Rubber absorbance to be measured, substitute into step 4) in the regression curve that draws, obtain halogenated butyl rubber and account for sky
So glue and percentage by weight of halogenated butyl rubber summation.
The assay method of the present invention is carried out checking test.Utilize known chlorinated butyl rubber and natural gum quality
The rubber of percentage ratio is verified, wherein the mass ratio of chlorinated butyl rubber and natural gum be 70% and
100%, the result utilizing the assay method of the present invention to obtain is 72.2% and 104.1%.
In the absorbance spectrum measured on infrared spectrometer, determine the target representing halogenated butyl rubber feature
The wave number at peak is at 1250cm-1～1220cm-1Between occur peak value, in test example 1, wave number is
1230cm-1Peak value.
Either brominated butyl rubber or chlorinated butyl rubber are difficult to natural gum in pyrolysis gas chromatography
Isolating characteristic peak, the target peak after the present invention utilizes infrared spectrometry to determine polymer cracking more holds
Easily.Halogenated butyl rubber and natural gum cracking afterproduct, the absworption peak quantity of functional group in infrared spectrogram
Few, and regular follow, and the characteristic peak of difference halogenated butyl rubber and natural gum is more apparent.
The present invention can summarize with other the concrete form without prejudice to the spirit or essential characteristics of the present invention.
Therefore, no matter from the point of view of which point, the embodiment above of the present invention all can only be considered the present invention's
Illustrating and can not limit the present invention, claims indicate the scope of the present invention, and above-mentioned explanation is also
Do not point out the scope of the present invention, therefore, in the implication suitable with claims of the present invention and scope
Any change, be all considered as being included in the range of claims of the present invention.
Claims (5)
1. in a rubber halogenated butyl rubber and natural gum and with than assay method, it is characterised in that
Step is as follows:
1) first application at least three contains the known rubber sample of halogenated butyl rubber and natural gum, with red
External spectrum instrument measures known rubber sample absorbance, calculates halogenated butyl rubber peak height value according to Formulas I and accounts for natural
Glue and the ratio of halogenated butyl rubber peak height value summation,
R=HA/(HA+HB) Formulas I
Wherein, HABe wave number be 1250cm-1～1220cm-1Between the peak of halogenated butyl rubber characteristic peak absorbance
High level, HBIt is that natural gum is at 885cm-1～889cm-1The peak height value of characteristic peak absorbance；
2) according to step 1) the R value that obtains, draw natural gum and halogenated butyl rubber shared by halogenated butyl rubber
The percentage duty curve of summation, particularly as follows: with R value as X-axis, with halogenated butyl rubber account for natural gum and
The percentage by weight of halogenated butyl rubber summation is Y-axis, draws regression curve with method of least square
Y=ax2+bx+c；
3) determination of infrared spectroscopy is utilized to contain the rubber absorbance to be measured of halogenated butyl rubber and natural gum,
Substitute into step 2) in the regression curve that draws, obtain halogenated butyl rubber and account for natural gum and halogenated butyl rubber is total
The percentage by weight of sum.
2. in rubber as claimed in claim 1 halogenated butyl rubber and natural gum and with than assay method,
It is characterized in that, the step of described determination of infrared spectroscopy known rubber sample absorbance includes:
1) extracting: by the B method of GB/T3516-2006, known rubber sample is stripped, and dries
Sample；
2) absorbance measurement: by step 1) in after extracting the sample that obtains, by cracking product after cracking
Thing infrared spectrometer records infrared spectrum in 2.5 μm～15 μ m wavelength range；Pyrolysis product is existed
Measure absorbance on infrared spectrometer, show that wave number is at 885cm-1～889cm-1And 1250cm-1~
1220cm-1Between peak height value.
3. in rubber as claimed in claim 2 halogenated butyl rubber and natural gum and with than assay method,
It is characterized in that, raw material and the parts by weight thereof of described known rubber sample are: halogenated butyl rubber is with natural
The parts by weight of glue and be 100 parts, operate oily 10 weight portions, white carbon black 70 weight portion, age resistor 1 weight
Amount part, sulfur 1 weight portion, zinc oxide 2 weight portion, accelerator 0.6 weight portion.
4. in rubber as claimed in claim 3 halogenated butyl rubber and natural gum and with than assay method,
It is characterized in that, described halogenated butyl rubber with the percentage by weight of natural gum is: 0:100,20:80,
40:60,50:50,60:40,70:30,80:20 or 100:0.
5. in rubber as claimed in claim 2 halogenated butyl rubber and natural gum and with than assay method,
It is characterized in that, described extracting, particularly as follows: extraction solvent is acetone, extracts 12h under 75 DEG C of water bath condition
After, change an acetone reagent, again extract 12h under 75 DEG C of water bath condition, put into after sample is taken out
105 DEG C of baking ovens dry to constant weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610281180.4A CN105891140A (en) | 2016-04-29 | 2016-04-29 | Method for measuring blending ratio of halogenated butyl rubber and natural rubber in rubber |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610281180.4A CN105891140A (en) | 2016-04-29 | 2016-04-29 | Method for measuring blending ratio of halogenated butyl rubber and natural rubber in rubber |
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|---|---|
| CN105891140A true CN105891140A (en) | 2016-08-24 |
Family
ID=56703286
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| CN201610281180.4A Pending CN105891140A (en) | 2016-04-29 | 2016-04-29 | Method for measuring blending ratio of halogenated butyl rubber and natural rubber in rubber |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1308231A (en) * | 2001-02-28 | 2001-08-15 | 中国石化集团扬子石油化工有限责任公司 | Fast test method of ethylene-propylene rubber content in ethylene-propylene copolymer |
| CN1655582A (en) * | 2004-02-12 | 2005-08-17 | 施乐公司 | System and method for connecting regions of image data having similar characteristics |
-
2016
- 2016-04-29 CN CN201610281180.4A patent/CN105891140A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1308231A (en) * | 2001-02-28 | 2001-08-15 | 中国石化集团扬子石油化工有限责任公司 | Fast test method of ethylene-propylene rubber content in ethylene-propylene copolymer |
| CN1655582A (en) * | 2004-02-12 | 2005-08-17 | 施乐公司 | System and method for connecting regions of image data having similar characteristics |
Non-Patent Citations (3)
| Title |
|---|
| 周淑华: "红外光谱法分析橡胶制品成分", 《光谱仪器与分析》 * |
| 王国强 等: "NR/SBR硫化胶的傅里叶变换红外光谱-计算机定量分析", 《合成橡胶工业》 * |
| 王锐兰 等: "红外光谱法鉴定并用橡胶成分", 《浙江化工》 * |
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