CN109270175A - Resin analyzes and identifies method in a kind of vulcanized rubber - Google Patents
Resin analyzes and identifies method in a kind of vulcanized rubber Download PDFInfo
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- CN109270175A CN109270175A CN201810938452.2A CN201810938452A CN109270175A CN 109270175 A CN109270175 A CN 109270175A CN 201810938452 A CN201810938452 A CN 201810938452A CN 109270175 A CN109270175 A CN 109270175A
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- resin
- vulcanized rubber
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
Abstract
What the present invention disclosed resin in a kind of vulcanized rubber analyzes and identifies method, comprising the following steps: shreds cured rubber samples and obtains extract liquor with solvent extraction, extract liquor is concentrated to dryness, toluene is added, ultrasonic vibration dissolves concentrate, obtains prepare liquid；Prepare liquid is placed in cracking instrument, 280 DEG C are warming up to, using inert gas purge sample 5min；Pintsch process detects the mass spectrum of the prepare liquid using gas chromatograph-mass spectrometer (GC-MS)；Corresponding monomer or oligomer ingredient are identified by corresponding mass spectrogram, the parsing of mass spectrogram is to determine corresponding resin types by standard spectrum library (NIST composes library) retrieval.The present invention is based on pyrolysis technologies and Gc/ms Analyser technology, obtain corresponding pyrogram, are identified by corresponding mass spectrogram corresponding monomer or oligomer ingredient, are suitable for vulcanized rubber, such as analyze and identify resin types in tire formulation.
Description
Technical field
The present invention relates to vulcanized rubber formulation analysis field, the side of analyzing and identifying of resin in specifically a kind of vulcanized rubber
Method, the instrument used are Gc/ms Analyser.
Background technique
With the development of industry, rubber product is widely used in industrial every field, and it is important to become industry
Raw material sources.Since vulcanized rubber is in sides such as constant glutinous, wearability, tensile strength, stretching strength, elongation, elasticity, hardness
There is excellent performance in face, so most of rubber products all use vulcanized rubber.Tire is usually by rubber system, vulcanization body
The composition that the multicomponents such as system, reinforcement system, preventing aging system cooperatively form.Resin is also important with being combined in the balanced constant
/ mono-, the service performance of tire and processing performance are influenced very big.The analysis method of resin types is for wheel in tire formulation
The control of tire quality, tire formulation research are of great significance.But at present also for the analysis method of resin types in tire formulation
Without effective solution, relevant report there are no.The application is based on pyrolysis technology and the realization pair of gas chromatography-mass spectrum technology
The test analysis of resin types in tire formulation.
Summary of the invention
It is an object of the invention to overcome defect of the existing technology, the analysis for providing resin in a kind of vulcanized rubber is surveyed
Identification method.
The purpose of the present invention can be achieved through the following technical solutions:
Resin analyzes and identifies method in a kind of vulcanized rubber, comprising the following steps:
(1) resin extracts: cured rubber samples being shredded, makes its size no more than 2cm*2cm, is extracted with solvent extraction
Liquid is taken, extract liquor is concentrated to dryness, toluene is added, ultrasonic vibration dissolves concentrate, obtains prepare liquid；
(2) high-temperature blowing: prepare liquid is placed in cracking instrument, 280 DEG C are warming up to, using helium purge sample 5min；
(3) test: Pintsch process detects the mass spectrum of the prepare liquid using gas chromatograph-mass spectrometer (GC-MS)；
Wherein, mass spectrographic condition is detected are as follows: EI ion source, 150 DEG C of level four bars temperature, scans model by 230 DEG C of ion source temperature
Enclose 50-350amu；
(4) it analyzes: corresponding monomer or oligomer ingredient being identified by corresponding mass spectrogram, the parsing of mass spectrogram
It is that corresponding resin types are determined by standard spectrum library (NIST composes library) retrieval.
Further scheme, extractant is selected from least one of alcohol, ketone, ether, aromatic hydrocarbons in the step (1).
Further scheme, the type of resin includes but is not limited to that styrene-α-methylstyrene is total in the vulcanized rubber
Poly resin, phenolic resin, DCPD resin, C5 resin, coumarone indene resin.
Further scheme, the middle cracking instrument of the step (2) is Curie point pyrolyzer.
Further scheme, inert gas is helium in the step (2).
Further scheme, step (3) the high temperature cracking temperature are 550 DEG C.
Further scheme, GC conditions in the step (3) are as follows: 5%- phenyl-methyl polysiloxanes capillary column,
300 DEG C of injector temperature；Carrier gas is He, flow velocity 1.0mL/min；Temperature programming condition: starting column temperature is 50 DEG C, is kept
2min is warming up to 280 DEG C with 10 DEG C/min, keeps 10min；Injection port split ratio is 30:1.
Vulcanized rubber is a kind of crosslinked cooperatively formed by multicomponent.It is ground through the experiment to common resins in rubber processing
Study carefully, mainly includes styrene-α-methylstyrene copolymer resins, DCPD resin, C5 resin, coumarone indene resin, phenolic resin, tree
The cross-linking reaction of rouge not fully, can be extracted by high-temperature pressurizing and be extracted.And rubber matrix after crosslinking due to forming
Crosslinked can only be swollen, and cannot be dissolved again, therefore will not be extracted in high-temperature extraction.
In addition to the resin component of extraction in vulcanized rubber extract liquor, while also containing auxiliary component used in cooperation, one
As include wax, anti-aging agent, oil, promotor decomposition product and other compounding aids.Identification point of these non-resin ingredients to resin
Analysis has very big interference, needs to be further purified.This programme is mainly using the otherness decomposed with volatilization temperature, by under high temperature
Inert gas purge makes these interference components volatilize or decompose.
Through to resin Pintsch process characteristic research and literature survey, the decomposition temperature of resin component is higher, such as C5 resin
Initial decomposition temperature be 280 DEG C or so.By thermogravimetic analysis (TGA) (TGA), 10min under resin maintains at a high temperature of 300 DEG C,
The decomposition of resin is still limited, and in the resin analyzed, maximum decomposition amount is also no more than 40%, and surveys in actual analysis
In examination, purge time is shorter, and practical decomposition amount can be smaller.
Compared with resin, the molecular weight of auxiliary molecules is typically small, is easy to happen volatilization at high temperature, therefore to temperature
Rationally control can be such that the volatilization of low molecular weight auxiliary component removes, while can be reduced the decomposition of resin and retain most tree
Rouge ingredient.
Beneficial effects of the present invention:
1, the present invention is based on pyrolysis technologies and Gc/ms Analyser technology, obtain corresponding pyrogram,
Corresponding monomer or oligomer ingredient are identified by corresponding mass spectrogram, is suitable for vulcanized rubber, such as analyzes and identifies wheel
Resin types in tire formula.
2, the present invention makes these interference by inert gas purge under high temperature using the otherness of decomposition and volatilization temperature
Ingredient volatilization is decomposed, while be can be reduced the decomposition of resin and being retained most resin component.
3, the present invention extracts resin using high temperature and high pressure from vulcanized rubber, cannot using the crosslinking feature of rubber matrix
It dissolves, resin is separated with rubber matrix.
Detailed description of the invention
Fig. 1 is the chromatogram of resin analysis in embodiment 1.
Fig. 2 is the corresponding mass spectrogram of chromatographic peak in embodiment 1.
Fig. 3 is blank control spectrogram in embodiment 2 (SBR vulcanized rubber is free of resin component).
Fig. 4 is the SBR vulcanized rubber pyrogram of styrene methyl styrene copolymerized resin in embodiment 2.
Fig. 5 is α-methylstyrene mass spectrogram in embodiment 2 (source EI).
Label in Fig. 4: 1- air background peak, 2- cyclopentadiene, 3- methyl cyclopentadiene, 4- toluene, 5- ethylbenzene, 6- benzene second
Alkene, 7- α-methylstyrene.
Fig. 6 is styrene styrene mass spectrogram (source EI) in embodiment 2.
Fig. 7 is the chromatogram of resin analysis in embodiment 3.
Fig. 8 is the corresponding mass spectrogram of chromatographic peak (source EI) in embodiment 3
Fig. 9 is the chromatogram of resin analysis in embodiment 4.
Figure 10 is the corresponding mass spectrogram of chromatographic peak (source EI) in embodiment 4.
Specific embodiment
Present invention is further described in detail in the following with reference to the drawings and specific embodiments.
Instrument and reagent
Reagent: toluene, acetone are analytical reagents
Instrument: Accelerate solvent extraction instrument: U.S. ThermoFisher AES100；
Gas chromatograph-mass spectrometer (GC-MS): U.S. Agilent 7890A-5975C；
Thermal cracking instrument: U.S. CDS 5150；
Ultrasonic vibration instrument；
Electronic balance sartorius BSA124S (sensibility reciprocal 0.1mg)
Embodiment 1
The present embodiment is that dicyclopentadiene novolacs (DCPD resin) analyzes and identifies in tire formulation.Specifically include following step
It is rapid:
1, resin extracts
Tyre vulcanization rubber 5g to be analyzed is taken, is shredded, makes its size no more than 2cm*2cm.Place it in stainless steel
In abstraction pool, the resin component in tyre vulcanization rubber is extracted using Accelerate solvent extraction instrument.Extract liquor is transferred to round bottom to burn
It in bottle, is concentrated to dryness, 1ml toluene solvant is added, ultrasonic vibration 10min dissolves concentrate, as subsequent prepare liquid.With
Under be design parameter used by Accelerate solvent extraction instrument:
Extractant: acetone
Extraction time: 2*30min
Extraction temperature: 100 DEG C
Extractant volume: 60ml
2, the identification of resin component
Mineral wool is added in the sample cell of thermal cracking instrument, takes 20ul to be slowly added in sample cell above-mentioned prepare liquid
On mineral wool, the mineral wool being added in sample cell should prevent prepare liquid exudation (can also take the mode being added by several times) enough；
By above-mentioned sample cell naturally dry (or use and be dried with nitrogen), then sample cell is placed in be analyzed in thermal cracking instrument；Thermal cracking
Instrument is warming up to 280 DEG C, using helium purge sample 5min, is then rapidly heated and cracks resin to 550 DEG C, cracking gas is led automatically
Enter in gas chromatograph-mass spectrometer (GC-MS) and analyzes.
The following are the specific experiment parameters of thermal cracking instrument and gas chromatograph-mass spectrometer (GC-MS):
Each main chromatographic peak is given by corresponding mass spectrogram qualitative, phase is determined according to the monomer of cracking or oligomer
The resin types answered.Fig. 1 is the chromatogram of resin analysis, and Fig. 2 is the corresponding mass spectrogram of chromatographic peak.It is true by NIST library searching
Main peaks are cyclopentadiene in the fixed vulcanized rubber sample analysis spectrogram.It can be determined in the vulcanized rubber according to the monomer
Resin types are DCPD resinoid.
The explanation of DCPD resin: DCPD resin (Dicyclopentadiene petroleum resin), is by pentamethylene
The Petropols that the dimer dicyclopentadiene of diene polymerize at high temperature under high pressure.So the list formed after polymer cracking
Body is cyclopentadiene, so that it may determine that resin is DCPD Petropols.
Embodiment 2
The present embodiment is that the analyzing and identifying of styrene resin and DCPD resin in tire formulation (two kinds of resins while containing
Have).Its main rubber is SBR vulcanized rubber.
1, resin extracts
Tyre vulcanization rubber 5g to be analyzed is taken, is shredded, makes its size no more than 2cm*2cm.Place it in stainless steel
In abstraction pool, the resin component in tyre vulcanization rubber is extracted using Accelerate solvent extraction instrument.Extract liquor is transferred to round bottom to burn
It in bottle, is concentrated to dryness, 1ml toluene solvant is added, ultrasonic vibration 10min dissolves concentrate, as subsequent prepare liquid.With
Under be design parameter used by Accelerate solvent extraction instrument:
Extractant: acetone
Extraction time: 2*30min
Extraction temperature: 100 DEG C
Extractant volume: 60ml
2, the identification of resin component
Mineral wool is added in the sample cell of thermal cracking instrument, takes 20ul to be slowly added in sample cell above-mentioned prepare liquid
On mineral wool, the mineral wool being added in sample cell should prevent prepare liquid exudation (can also take the mode being added by several times) enough；
By above-mentioned sample cell naturally dry (or use and be dried with nitrogen), then sample cell is placed in be analyzed in thermal cracking instrument；Thermal cracking
Instrument is warming up to 280 DEG C, using helium purge sample 5min, is then rapidly heated and cracks resin to 550 DEG C, cracking gas is led automatically
Enter in gas chromatograph-mass spectrometer (GC-MS) and analyzes.
The following are the specific experiment parameters of thermal cracking instrument and gas chromatograph-mass spectrometer (GC-MS):
Each main chromatographic peak is given by corresponding mass spectrogram qualitative, phase is determined according to the monomer of cracking or oligomer
The resin types answered.
Since part uncrosslinked in butadiene-styrene rubber can be equally extracted, styrene list can be similarly generated after cracking
Body, but its cracking peak generated is smaller compared with the cracking peak of benzene Class B olefine resin, does not influence analyzing and identifying for resin.Fig. 3 is
Styrene-butadiene vulcanized rubber analysis of spectra without resin component, reasons for its use peak very little.
Embodiment vulcanized rubber analysis chromatogram is shown in Fig. 4, determines that monomer is ring by corresponding mass-spectrogram library searching
Pentadiene, styrene, α-methylstyrene contain DCPD resin, styrene-Alpha-Methyl benzene second in the deducibility vulcanized rubber
Olefine resin.
Styrene-α-methylstyrene resin explanation: styrene-α-methylstyrene copolymer resins be by styrene and
Polymer made of α-methylstyrene copolymerization.Therefore so the monomer formed after polymer cracking is styrene and Alpha-Methyl benzene
Ethylene, so that it may determine that resin is styrene-α-methylstyrene resin.
Embodiment 3
The present embodiment is that styrene-butadiene resins analyze and identify in tire formulation.Its main rubber is SBR vulcanization
Rubber.
1, resin extracts
Tyre vulcanization rubber 5g to be analyzed is taken, is shredded, makes its size no more than 2cm*2cm.Place it in stainless steel
In abstraction pool, the resin component in tyre vulcanization rubber is extracted using Accelerate solvent extraction instrument.Extract liquor is transferred to round bottom to burn
It in bottle, is concentrated to dryness, 1ml toluene solvant is added, ultrasonic vibration 10min dissolves concentrate, as subsequent prepare liquid.With
Under be design parameter used by Accelerate solvent extraction instrument:
Extractant: acetone
Extraction time: 2*30min
Extraction temperature: 100 DEG C
Extractant volume: 60ml
2, the identification of resin component
Mineral wool is added in the sample cell of thermal cracking instrument, takes 20ul to be slowly added in sample cell above-mentioned prepare liquid
On mineral wool, the mineral wool being added in sample cell should prevent prepare liquid exudation (can also take the mode being added by several times) enough；
By above-mentioned sample cell naturally dry (or use and be dried with nitrogen), then sample cell is placed in be analyzed in thermal cracking instrument；Thermal cracking
Instrument is warming up to 280 DEG C, using helium purge sample 5min, is then rapidly heated and cracks resin to 550 DEG C, cracking gas is led automatically
Enter in gas chromatograph-mass spectrometer (GC-MS) and analyzes.
The following are the specific experiment parameters of thermal cracking instrument and gas chromatograph-mass spectrometer (GC-MS):
Each main chromatographic peak is given by corresponding mass spectrogram qualitative, phase is determined according to the monomer of cracking or oligomer
The resin types answered.Fig. 7 is the chromatogram of resin analysis, and Fig. 8 is the corresponding mass spectrogram of chromatographic peak.It is true by NIST library searching
Main peaks are butadiene, butadiene dimer and styrene in the fixed vulcanized rubber sample analysis spectrogram.According to the monomer and
Oligomer can determine that the resin types in the vulcanized rubber are styrene butadiene copolymers resin.
The explanation of styrene-butadiene resins: styrene and butadiene resin are the copolymerization trees by styrene and butadiene
Rouge.So the monomer formed after polymer cracking is styrene and butadiene and its oligomer, so that it may determine that the resin is benzene
Ethylene and butadiene copolymer resin.
Note: the polymerized monomer and butadiene-styrene rubber of the resinoid are all butadiene and styrene, but its molecular weight is relatively low,
Generally 2000-3000 (and the number-average molecular weight of butadiene-styrene rubber is then generally 10-40 ten thousand)；The resinoid in vulcanized rubber can
To be analyzed and identified using this method.
Embodiment 4
The present embodiment is that phenolic resinoid analyzes and identifies in tire formulation.
1, resin extracts
Tyre vulcanization rubber 5g to be analyzed is taken, is shredded, makes its size no more than 2cm*2cm.Place it in stainless steel
In abstraction pool, the resin component in tyre vulcanization rubber is extracted using Accelerate solvent extraction instrument.Extract liquor is transferred to round bottom to burn
It in bottle, is concentrated to dryness, 1ml toluene solvant is added, ultrasonic vibration 10min dissolves concentrate, as subsequent prepare liquid.With
Under be design parameter used by Accelerate solvent extraction instrument:
Extractant: acetone
Extraction time: 2*30min
Extraction temperature: 100 DEG C
Extractant volume: 60ml
2, the identification of resin component
Mineral wool is added in the sample cell of thermal cracking instrument, takes 20ul to be slowly added in sample cell above-mentioned prepare liquid
On mineral wool, the mineral wool being added in sample cell should prevent prepare liquid exudation (can also take the mode being added by several times) enough；
By above-mentioned sample cell naturally dry (or use and be dried with nitrogen), then sample cell is placed in be analyzed in thermal cracking instrument；Thermal cracking
Instrument is warming up to 280 DEG C, using helium purge sample 5min, is then rapidly heated and cracks resin to 550 DEG C, cracking gas is led automatically
Enter in gas chromatograph-mass spectrometer (GC-MS) and analyzes.
The following are the specific experiment parameters of thermal cracking instrument and gas chromatograph-mass spectrometer (GC-MS):
Each main chromatographic peak is given by corresponding mass spectrogram qualitative, phase is determined according to the monomer of cracking or oligomer
The resin types answered.Fig. 9 is the chromatogram of analysis, and Figure 10 is the corresponding mass spectrogram of chromatographic peak.It is determined by NIST library searching
Main peaks are phenol in the vulcanized rubber sample analysis spectrogram.The resin kind in the vulcanized rubber can be determined according to the monomer
Class is phenolic resinoid.
Note: thermoplastic phenolic resin is only applicable to for phenolic resinoid, is not suitable for heat cured resin.
This hair can be understood and applied the above description of the embodiments is intended to facilitate those skilled in the art
It is bright.Person skilled in the art obviously easily can make various modifications to case study on implementation, and described herein one
As principle be applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to implementation cases here
Example, those skilled in the art's announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be
Within protection scope of the present invention.
Claims (7)
1. resin analyzes and identifies method in a kind of vulcanized rubber, which comprises the following steps:
(1) resin extracts: cured rubber samples being shredded, makes its size no more than 2cm*2 cm, is extracted with solvent extraction
Extract liquor is concentrated to dryness by liquid, and toluene is added, and ultrasonic vibration dissolves concentrate, obtains prepare liquid；
(2) high-temperature blowing: prepare liquid is placed in cracking instrument, 280 DEG C are warming up to, using inert gas purge sample 5min；
(3) test: Pintsch process detects the mass spectrum of the prepare liquid using gas chromatograph-mass spectrometer (GC-MS)；
Wherein, mass spectrographic condition is detected are as follows: EI ion source, 230 DEG C of ion source temperature, 150 DEG C of level four bars temperature, scanning range
50-350amu；
(4) it analyzes: corresponding monomer or oligomer ingredient being identified by corresponding mass spectrogram, the parsing of mass spectrogram is logical
Standard spectrum library (NIST composes library) retrieval is crossed, determines corresponding resin types.
2. resin analyzes and identifies method in vulcanized rubber according to claim 1, which is characterized in that the step (1)
Middle extractant is selected from least one of alcohol, ketone, ether, aromatic hydrocarbons.
3. resin analyzes and identifies method in vulcanized rubber according to claim 1, which is characterized in that the vulcanized rubber
The type of middle resin include but is not limited to styrene-α-methylstyrene copolymer resins, phenolic resin, DCPD resin, C5 resin,
Coumarone indene resin.
4. resin analyzes and identifies method in vulcanized rubber according to claim 1, which is characterized in that the step (2)
Middle cracking instrument is Curie point pyrolyzer.
5. resin analyzes and identifies method in vulcanized rubber according to claim 1, which is characterized in that the step (2)
Middle inert gas is helium.
6. resin analyzes and identifies method in vulcanized rubber according to claim 1, which is characterized in that the step (3)
High temperature cracking temperature is 550 DEG C.
7. resin analyzes and identifies method in vulcanized rubber according to claim 1, which is characterized in that the step (3)
Middle GC conditions are as follows: 5%- phenyl-methyl polysiloxanes capillary column, 300 DEG C of injector temperature；Carrier gas is He, flow velocity is
1.0 mL/min；Temperature programming condition: starting column temperature is 50 DEG C, keeps 2min, is warming up to 280 DEG C with 10 DEG C/min, keeps 10
min；Injection port split ratio is 30:1.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112730648A (en) * | 2020-12-09 | 2021-04-30 | 中国刑事警察学院 | Determination of content of p-phenylenediamine anti-aging agent in rubber by pyrolysis gas chromatography mass spectrometer |
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| US20160103106A1 (en) * | 2014-10-09 | 2016-04-14 | Shimadzu Corporation | Reference sample for analysis |
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| JPH01229963A (en) * | 1988-03-10 | 1989-09-13 | Mitsubishi Petrochem Co Ltd | Thermal-decomposition gaschromatography |
| US20160103106A1 (en) * | 2014-10-09 | 2016-04-14 | Shimadzu Corporation | Reference sample for analysis |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112730648A (en) * | 2020-12-09 | 2021-04-30 | 中国刑事警察学院 | Determination of content of p-phenylenediamine anti-aging agent in rubber by pyrolysis gas chromatography mass spectrometer |
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Application publication date: 20190125 |