CN104251794A - Making method and making apparatus of rubber product - Google Patents
Making method and making apparatus of rubber product Download PDFInfo
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- CN104251794A CN104251794A CN201310258180.9A CN201310258180A CN104251794A CN 104251794 A CN104251794 A CN 104251794A CN 201310258180 A CN201310258180 A CN 201310258180A CN 104251794 A CN104251794 A CN 104251794A
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Abstract
The invention provides a making method and a making apparatus of a rubber product. The making method comprises the following steps: sequentially placing the extracted rubber product and a selected solvent in a closed space; heating to maintain the closed space at a predetermined temperature within a predetermined time to make the rubber molecules of the extracted rubber product dissolved in the selected solvent through a reverse reaction of a cross-linking reaction in order to form a rubber dissolution liquid; and filtering the rubber dissolution liquid, making a sample to be analyzed, and carrying out fine analysis on the rubber molecules through infrared spectroscopic analysis or liquid chromatographic analysis due to the complete reservation of rubber molecule chains in the sample to be analyzed.
Description
Technical field
The present invention relates to material analysis field, particularly relate to a kind of method for making sample and sample making apparatus of rubber.
Background technology
Identification and analysis is carried out for rubber types in existing rubber and portions additive, usually uses infrared spectroscopy, then usually liquid phase chromatography is used to the mensuration of rubber molecular chain size distribution.Because the rubber overwhelming majority is vulcanized rubber, rubber molecule forms stereoeffect therein after sulfuration generation cross-linking reaction, based on Infrared spectroscopy and liquid-phase chromatographic analysis to the particular/special requirement of sample state, needed to carry out sample preparation to rubber before carrying out Infrared spectroscopy or liquid-phase chromatographic analysis to rubber, to form the sample to be analyzed meeting and analyze and require.
In prior art, in view of rubber is difficult to the characteristic being dissolved in solvent usually, take cracking process to carry out sample preparation more.Cracking process sample preparation generally comprises following steps: carry out extracting to rubber, to remove solvable adjuvant; Heating pyrolyze is carried out to the rubber after extracting, extracts lysate; Use lysate film, to form sample to be analyzed.But use cracking process to prepare sample existing defects to be analyzed: because rubber is high molecular polymer, the strand generation random fracture of rubber when cracking, and fracture after occur again random combine formed pyrolysis product, therefore pyrolysis product and former rubber true molecular textural difference very large.The reason that there are the problems referred to above is, during rubber molecule generation cracking, pyrolysis product, with cracking condition (as temperature) change, uncontrollable change occurs; Even if under stable cracking condition, as constant temperature cracking, the random combine of the random fracture of the rubber raw materials strand still after uncontrollable cracking and the rear strand fragment of fracture.Therefore, substantially former rubber molecule structure can not be reproduced in the sample to be analyzed using existing cracking process sample preparation to obtain, the kind of rubber raw materials can only be judged according to certain the intrinsic segment molecule chain in pyrolysis product, so the sample to be analyzed that cracking process sample preparation obtains also can only carry out rubber types qualification and not analyze rubber molecule structure by Infrared spectroscopy, the quantitative measurement of rubber molecular chain size distribution can not be carried out to rubber molecule by liquid phase chromatography, therefore, existing method for making sample cannot meet the requirement of rubber molecule explication de texte.
Summary of the invention
The invention provides a kind of rubber method for making sample and sample making apparatus, the sample to be analyzed obtained to solve existing cracking process sample preparation can not meet the problem required rubber molecule explication de texte.
For solving the problem, the invention provides a kind of method for making sample of rubber, comprising:
Extracting is carried out to rubber, to remove the solvable adjuvant in rubber;
Rubber after extracting and selected solvent are placed in confined space;
Making confined space keep predetermined temperature in the given time by heating confined space, to be dissolved in selected solvent by the reversed reaction of cross-linking reaction to make the rubber molecule in the rubber after extracting and to form rubber solvent;
Rubber solvent is filtered, to remove the solid residue in rubber solvent;
The rubber solvent after filtering is used to make sample to be analyzed.
Further, described selected solvent is toluene or chlorobenzene.
Further, the volume of described selected solvent is 2 to 5 milliliters, and the rubber weight after described extracting is 0.1 to 0.5 gram.
Further, the described schedule time is greater than 100 minutes, and predetermined temperature is not higher than 250 DEG C.
Further, the described schedule time is 120 minutes, and predetermined temperature is 250 DEG C.
Further, described rubber solvent is filtered before, this method for making sample carries out extracting to absorbent cotton further, to remove the impurity in absorbent cotton; And, describedly filtration is carried out to rubber solvent comprise: utilize the absorbent cotton after extracting to filter rubber solvent.
Further, use the rubber solvent after filtering to make sample to be analyzed to comprise:
Rubber solvent after filtering is concentrated, to remove the described selected solvent in lysate; Use the rubber solvent film after concentrated described filtration, obtain sample to be analyzed;
Or, quantitatively transfer is diluted to the rubber solvent after filtering, obtains sample to be analyzed.
Further, described carried out to the rubber solvent after filtering concentrated comprising: the rubber solvent after filtering is toasted, and rubber solvent volume after filtration toasts after adding spectroscopic pure acetone after reducing 1/4 again.
Present invention also offers a kind of sample making apparatus of rubber, it is characterized in that, comprising:
Rubber extracting parts, for carrying out extracting to rubber, to remove the solvable adjuvant in rubber;
Closed container parts, for providing confined space and rubber in confined space after accommodating extracting and selected solvent;
High-temperature heating parts, keep predetermined temperature in the given time for heating, make confined space to confined space, to be dissolved in selected solvent by the reversed reaction of cross-linking reaction to make the rubber molecule in the rubber after extracting and to form rubber solvent;
Solution filter element, for filtering lysate, to remove the solid residue in rubber solvent;
Sample making parts to be analyzed, make sample to be analyzed for using the rubber solvent after filtration.
Further, described closed container parts are molten sample pipe, and this molten sample pipe comprises sealing-plug and instrumentation tubes; Wherein, one end sealing of described instrumentation tubes, the other end are provided with opening, and the opening of described instrumentation tubes and described sealing-plug are tightly connected by threaded engagement;
Described high-temperature heating parts comprise heating board and the heating module be arranged in described heating board and control module; Wherein, described heating board is provided with the bottoming hole holding described molten sample pipe, and described heating module is used for heating described bottoming hole, and described control module is for controlling heat time and the heating-up temperature of described heating module.
Further, the sample making apparatus of rubber also comprises absorbent cotton extracting parts; Described solution filter element is the absorbent cotton after extracting.
Further, described sample making parts to be analyzed comprise solution condensation means and are coated with membrane element, and wherein said solution condensation means is used for the rubber solvent after thickening filtration, and described painting membrane element is used for the rubber solvent film after by concentrated described filtration;
Or described sample making parts to be analyzed comprise and quantitatively dilute transfering part, for quantitatively diluting transfer to the rubber solvent after filtering.
Adopt rubber method for making sample provided by the invention and sample making apparatus, rubber after extracting and selected solvent are placed in confined space, confined space is made to keep predetermined temperature in the given time by carrying out heating, to be dissolved in selected solvent by the reversed reaction of cross-linking reaction to make the rubber molecule in the rubber after extracting and to form rubber solvent, after rubber solvent is filtered, making sample to be analyzed; Due in formation sample to be analyzed, rubber molecule is directly dissolved in solvent, so the rubber molecule structure in sample to be analyzed retains complete, therefore, carries out explication de texte by Infrared spectroscopy or liquid-phase chromatographic analysis to rubber molecule.
Accompanying drawing explanation
Fig. 1 is the process flow diagram of a kind of rubber method for making sample of the present invention;
Fig. 2 is the structural representation of molten sample pipe in rubber sample making apparatus of the present invention;
Fig. 3 is the structural representation of well heater in rubber sample making apparatus of the present invention.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, to develop simultaneously embodiment referring to accompanying drawing, the present invention is described in further detail.
The present invention realizes based on following principle:
Rubber has the characteristic because absorbing particular liquid generation volumetric expansion, and therefore the dissolving of rubber also can regard the result of infinite swelling as; For the rubber after cross-linking reaction occurs because of sulfuration, swelling can only proceed to a certain degree till, namely there is the characteristic of limited swelling.According to above-mentioned character, applicant finds in high-temperature solvent, and rubber infinite swelling can occur, and the final reversed reaction that cross-linking reaction occurs, makes rubber molecule be dissolved in solvent.
Utilize above-mentioned principle, the rubber molecular chain in rubber can not be destroyed, rubber molecule is directly dissolved in solvent, the lysate being dissolved with rubber molecule is made into sample to be analyzed, then can carry out explication de texte to rubber molecule by infrared spectroscopy or liquid phase chromatographic analysis method.
Based on above-mentioned design, the invention provides a kind of method for making sample of rubber, as shown in Figure 1, comprising:
Extracting is carried out to rubber, to remove the solvable adjuvant in rubber;
Rubber after extracting and selected solvent are placed in confined space;
Making confined space keep predetermined temperature in the given time by heating confined space, to be dissolved in selected solvent by the reversed reaction of cross-linking reaction to make the rubber molecule in the rubber after extracting and to form rubber solvent;
Rubber solvent is filtered, to remove the solid residue in rubber solvent;
The rubber solvent after filtering is used to make sample to be analyzed.
Below in conjunction with the exemplary embodiments of the method for making sample of a kind of rubber of the present invention, method for making sample of the present invention is described in detail:
When carrying out sample preparation, first, extracting is carried out to rubber, to remove the solvable adjuvant in rubber, the rubber after extracting and selected solvent are placed in confined space, wherein, selected solvent is the polarity or intensive polar solvent that high thermal stability, volatility are moderate, preferred toluene or chlorobenzene, be preferably 0.1 to 0.5 gram for the rubber weight making sample to be analyzed, and the volume of selected solvent is 2 to 5 milliliters;
Then, making confined space keep predetermined temperature in the given time by heating confined space, to be dissolved in selected solvent by the reversed reaction of cross-linking reaction to make in the rubber after extracting rubber molecule and to form rubber solvent; Wherein, the schedule time is greater than 100 minutes, and predetermined temperature is not higher than 250 DEG C, and preferred as the present embodiment, the schedule time is 120 minutes, and predetermined temperature is 250 DEG C; By this step, because rubber there occurs the reversed reaction of cross-linking reaction under the condition of high-temperature solvent, rubber molecule is dissolved in solvent, and therefore, the rubber molecule comprised in the rubber solvent of formation has complete molecular structure;
Extracting is carried out to absorbent cotton, to remove the impurity in absorbent cotton, and utilizes the absorbent cotton after extracting to filter rubber solvent, to remove the solid residue in rubber solvent;
When making Infrared spectroscopy sample, further the rubber solvent after filtration is concentrated, preferably toast rubber solutions is concentrated to the rubber solvent after filtration, and rubber solvent volume after filtration toasts, again to remove the solvent in lysate after adding spectroscopic pure acetone after reducing 1/4;
Rubber solvent after concentrated is carried out film, forms sample to be analyzed;
When making liquid-phase chromatographic analysis sample, further quantitatively transfer being diluted to the rubber solvent after filtration, forming sample to be analyzed.
Method for making sample provided by the present invention be it should be noted that, first, although give the weight of rubber and selected liquor capacity in an embodiment, but do not limit the weight of rubber and selected solvent volume in the present invention, those skilled in the art can choose suitable parameter according to concrete analysis demand; Secondly, although the present embodiment only lists the method that rubber solutions that two kinds of utilizations are dissolved with rubber molecule makes sample to be analyzed, but, as general knowledge as well known to those skilled in the art, because different analytical approachs is different to the process of sample to be analyzed, for how to make sample to be analyzed by rubber solvent, those skilled in the art can utilize conventional techniques means to process the rubber solvent being dissolved with rubber molecule according to concrete analytical approach, make sample to be analyzed.
Present invention also offers a kind of sample making apparatus of rubber, comprising:
Rubber extracting parts, for carrying out extracting to rubber, to remove the solvable adjuvant in rubber;
Closed container parts, for providing confined space and rubber in confined space after accommodating extracting and selected solvent;
High-temperature heating parts, keep predetermined temperature in the given time for heating, make confined space to confined space, to be dissolved in selected solvent by the reversed reaction of cross-linking reaction to make the rubber molecule in the rubber after extracting and to form rubber solvent;
Solution filter element, for filtering lysate, to remove the solid residue in rubber solvent;
Sample making parts to be analyzed, make sample to be analyzed for using the rubber solvent after filtration.
Further, the sample making apparatus of rubber also comprises absorbent cotton extracting parts; Solution filter element is the absorbent cotton after extracting; When making Infrared spectroscopy sample, sample making parts to be analyzed comprise solution condensation means and are coated with membrane element, wherein solution condensation means is for the rubber solvent after thickening filtration, be coated with membrane element and be used for the rubber solvent film after by concentrated filtration, wherein, preferably use infrared lamp concentrated to rubber solvent baking; When making liquid-phase chromatographic analysis sample, sample making parts to be analyzed comprise and quantitatively dilute transfering part, for quantitatively diluting transfer to the rubber solvent after filtering.
Wherein, as preferred embodiment, with reference to Fig. 2 and Fig. 3, closed container parts are molten sample pipe 10, and this molten sample pipe 10 comprises sealing-plug 11 and instrumentation tubes 12; Wherein, one end sealing of instrumentation tubes 12, the other end are provided with opening (sign), and the opening of instrumentation tubes 12 is connected by screw thread 13 fitted seal with sealing-plug 11;
High-temperature heating parts 20 comprise the heating module 22 and control module (not shown) that heat board 21 and be arranged in heating board 21; Wherein, heating board 21 is provided with the bottoming hole 211 holding molten sample pipe 10, and heating module 22 is for heating bottoming hole 211, and control module is for controlling heat time and the heating-up temperature of heating module 22.
In sum, adopt rubber method for making sample provided by the invention and sample making apparatus, rubber after extracting and selected solvent are placed in confined space, confined space is made to keep predetermined temperature in the given time by carrying out heating, to be dissolved in selected solvent by the reversed reaction of cross-linking reaction to make the rubber molecule in the rubber after extracting and to form rubber solvent, after rubber solvent is filtered, making sample to be analyzed; Due in formation sample to be analyzed, rubber molecule is directly dissolved in solvent, so the rubber molecule structure in sample to be analyzed retains complete, therefore, carries out explication de texte by Infrared spectroscopy or liquid-phase chromatographic analysis to the molecule of rubber.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment made, equivalent replacement, improvement etc., all should be included within the scope of protection of the invention.
Claims (12)
1. a method for making sample for rubber, comprising:
Extracting is carried out to rubber, to remove the solvable adjuvant in rubber;
Rubber after extracting and selected solvent are placed in confined space;
Making confined space keep predetermined temperature in the given time by heating confined space, to be dissolved in selected solvent by the reversed reaction of cross-linking reaction to make the rubber molecule in the rubber after extracting and to form rubber solvent;
Rubber solvent is filtered, to remove the solid residue in rubber solvent;
The rubber solvent after filtering is used to make sample to be analyzed.
2. method for making sample according to claim 1, is characterized in that, described selected solvent is toluene or chlorobenzene.
3. method for making sample according to claim 2, is characterized in that, the volume of described selected solvent is 2 to 5 milliliters, and the rubber weight after described extracting is 0.1 to 0.5 gram.
4. method for making sample according to claim 1, is characterized in that, the described schedule time is greater than 100 minutes, and predetermined temperature is not higher than 250 DEG C.
5. method according to claim 4, is characterized in that, the described schedule time is 120 minutes, and predetermined temperature is 250 DEG C.
6. method for making sample according to claim 1, is characterized in that, described rubber solvent is filtered before, this method for making sample carries out extracting to absorbent cotton further, to remove the impurity in absorbent cotton; And, describedly filtration is carried out to rubber solvent comprise: utilize the absorbent cotton after extracting to filter rubber solvent.
7. method according to claim 1, is characterized in that, uses the rubber solvent after filtering to make sample to be analyzed and comprises:
Rubber solvent after filtering is concentrated, to remove the described selected solvent in lysate; Use the rubber solvent film after concentrated described filtration, obtain sample to be analyzed;
Or, quantitatively transfer is diluted to the rubber solvent after filtering, obtains sample to be analyzed.
8. method according to claim 7, it is characterized in that, described carried out to the rubber solvent after filtering concentrated comprising: the rubber solvent after filtering is toasted, and rubber solvent volume after filtration toasts after adding spectroscopic pure acetone after reducing 1/4 again.
9. a sample making apparatus for rubber, is characterized in that, comprising:
Rubber extracting parts, for carrying out extracting to rubber, to remove the solvable adjuvant in rubber;
Closed container parts, for providing confined space and rubber in confined space after accommodating extracting and selected solvent;
High-temperature heating parts, keep predetermined temperature in the given time for heating, make confined space to confined space, to be dissolved in selected solvent by the reversed reaction of cross-linking reaction to make the rubber molecule in the rubber after extracting and to form rubber solvent;
Solution filter element, for filtering lysate, to remove the solid residue in rubber solvent;
Sample making parts to be analyzed, make sample to be analyzed for using the rubber solvent after filtration.
10. sample making apparatus according to claim 9, is characterized in that,
Described closed container parts are molten sample pipe, and this molten sample pipe comprises sealing-plug and instrumentation tubes; Wherein, one end sealing of described instrumentation tubes, the other end are provided with opening, and the opening of described instrumentation tubes and described sealing-plug are tightly connected by threaded engagement;
Described high-temperature heating parts comprise heating board and the heating module be arranged in described heating board and control module; Wherein, described heating board is provided with the bottoming hole holding described molten sample pipe, and described heating module is used for heating described bottoming hole, and described control module is for controlling heat time and the heating-up temperature of described heating module.
11. sample making apparatus according to claim 9, is characterized in that, also comprise absorbent cotton extracting parts; Described solution filter element is the absorbent cotton after extracting.
12. sample making apparatus according to claim 9, it is characterized in that, described sample making parts to be analyzed comprise solution condensation means and are coated with membrane element, wherein said solution condensation means is used for the rubber solvent after thickening filtration, and described painting membrane element is used for the rubber solvent film after by concentrated described filtration;
Or described sample making parts to be analyzed comprise and quantitatively dilute transfering part, for quantitatively diluting transfer to the rubber solvent after filtering.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201310258180.9A CN104251794A (en) | 2013-06-26 | 2013-06-26 | Making method and making apparatus of rubber product |
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| CN201310258180.9A CN104251794A (en) | 2013-06-26 | 2013-06-26 | Making method and making apparatus of rubber product |
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| CN104251794A true CN104251794A (en) | 2014-12-31 |
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| CN201310258180.9A Pending CN104251794A (en) | 2013-06-26 | 2013-06-26 | Making method and making apparatus of rubber product |
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Application publication date: 20141231 |