CN105527194A - Method for detecting processability of rubber for tire - Google Patents
Method for detecting processability of rubber for tire Download PDFInfo
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Abstract
The invention relates to a method for detecting the processability of rubber for a tire. The detection steps of the method are as follows: (1) performing a Mooney viscosity test on the crude rubber sample by adopting a Mooney viscometer; (2) cutting the same raw rubber sample with similar Mooney viscosity value tested in the step (1), putting the raw rubber sample into a torque rheometer, and fitting a power law equation of the raw rubber sample: lg η ═ (a ± 0.03) lg γ + (B ± 0.06); (3) and (3) satisfying the power law equation of the raw rubber sample in the step (2), and then the rheological property of the rubber for the tire is qualified. Has the advantages that: the invention adopts a torque rheometer capillary extrusion method to detect raw rubber system materials with similar Mooney viscosity values, inspects the apparent viscosity of rubber under different shearing rates of mixing, extrusion and the like of an internal mixer in practical application, and compared with the prior method, the method has more accurate actual production results.
Description
Technical field
The present invention relates to a kind of tyre rubber detection method, particularly relate to a kind of detection method of tyre rubber processing characteristics.
Background technology
The index investigating synthetic rubber processing characteristics in tyre industry is the Mooney viscosity value of rubber, and the rubbery system material of the same race of different manufacturers, different batches, processing characteristics may there are differences in actual applications, causes the phenomenon off quality of glue stuff compounding.Be specially, because the test condition of Mooney viscosity value is single, temperature is 100 DEG C, rotor speed is 2r/min, namely shear rate is at about 1.31/s, but the temperature in actual production and shear rate are changes, and than Mooney viscosity test temperature and shear rate high, so the Mooney viscosity value measuring material under single condition can not the good usability of reaction material in process, the close different manufacturers of Mooney viscosity value is often there will be in actual production, or the rubber material of the same race of the different batches of same producer, glue stuff compounding Mooney viscosity differs greatly, there is the phenomenon of larger difference in processing characteristics.
Therefore, be necessary to propose effective technical scheme, solve the problem.
Summary of the invention
The present invention is directed to above-mentioned the deficiencies in the prior art, the detection method of the tyre rubber processing characteristics providing a kind of accuracy high.
The technical scheme that the present invention solves the problems of the technologies described above is as follows:
A detection method for tyre rubber processing characteristics, the detecting step of described method is as follows:
(1) mooney's viscosimeter is adopted to carry out Mooney viscosity test to rubber sample; Described rubber sample is selected from the product of the different batches that elastomeric different supplier of the same race or same provider provide; Described rubber sample is at least 50 groups;
(2) to after the close rubber sample of the same race cutting of the Mooney viscosity value tested out in step (1), torque rheometer is put into;
Torque rheometer inputs the rate of specific gravity of rubber sample, weighs and extrude quality, the numerical value of record shear viscosity and shear stress under each speed, according to the numerical value of shear rate and apparent shear viscosity, simulate the power-law equation of rubber sample;
Described power-law equation is as follows:
lgη＝(A±0.03)lgγ+(B±0.06)
In formula, η is apparent shear viscosity, and γ is shear rate, and A is n-1, and described n is non-newtonian index, and B is LgK, the apparent viscosity that described K is shear rate when being 0;
(3) meet the power-law equation of the described rubber sample of step (2), then the rheological property of described tyre rubber is qualified; Do not meet the power-law equation of the described rubber sample of step (2), then the rheological property of described tyre rubber is defective.
Preferably, described torque rheometer is Single screw extrusion, capillary die, the specification of capillary die is L/D=10, L/D=20, L/D=30, L/D=40, the rotating speed of extrusion screw rod is 1r/min ~ 30r/min, extrusion temperature is 110 DEG C ~ 170 DEG C, and each rate of extrusion lower retention time is 60s.
Preferably, described rubber sample is natural rubber or synthetic rubber; Described synthetic rubber is butadiene rubber, styrene-butadiene rubber, ethylene-propylene-diene rubber or butyl rubber.
Preferably, described styrene-butadiene rubber is solution polymerized butadiene styrene rubber or emulsion polymerized styrene butadiene rubber.Described solution polymerized butadiene styrene rubber is non-oil-filled solution polymerized butadiene styrene rubber or oil-filled solution polymerized butadiene styrene rubber, and described emulsion polymerized styrene butadiene rubber is non-oil-filled emulsion polymerized styrene butadiene rubber or oil-filled emulsion polymerized styrene butadiene rubber.
Preferably, described torque rheometer is mixing type torque rheometer.
Beneficial effect:
The present invention adopts torque rheometer kapillary extrusion method to detect the close rubber system material of Mooney viscosity value, investigate rubber in actual applications mixer mixing, the apparent viscosity of rubber under different shear rate such as to extrude, compared with the conventional method, the result of the method to actual production is more accurate.
For the corresponding equation of synthetic rubber matching of the same race of different manufacturers, different batches, detect the processing characteristics of this kind of material in actual production, the processing characteristics that the material meeting equation is considered to its elastomeric compound is close, adjusting process is not needed in following process process, do not meet the material of equation, although Mooney viscosity is close, in actual process, need the adjustment carrying out suitable process conditions.
Accompanying drawing explanation
Hereinafter describe specific embodiments more of the present invention with reference to the accompanying drawings by way of example, and not by way of limitation in detail.Reference numeral identical in accompanying drawing denotes same or similar parts or part.It should be appreciated by those skilled in the art that these accompanying drawings may not be drawn in proportion.In accompanying drawing:
Fig. 1 is the non-oil-filled shear viscosity of emulsion polymerized styrene butadiene rubber 1502 and the log-log graph of shear rate of the bright and beautiful lake petrochemical industry of the embodiment of the present invention 1;
Fig. 2 is the non-oil-filled shear viscosity of emulsion polymerized styrene butadiene rubber 1502 and the log-log graph of shear rate of the Qilu Petrochemical of the embodiment of the present invention 2;
Fig. 3 is the non-oil-filled shear viscosity of emulsion polymerized styrene butadiene rubber 1502 of raising sub-petrochemical industry and the log-log graph of shear rate of the embodiment of the present invention 3;
Fig. 4 is the non-oil-filled shear viscosity of emulsion polymerized styrene butadiene rubber 1502 and the log-log graph of shear rate of the Jilin Petrochemical of the embodiment of the present invention 4;
Fig. 5 is the oil-filled shear viscosity of solution polymerized butadiene styrene rubber 6270M and the log-log graph of shear rate of the bright and beautiful lake petrochemical industry of the embodiment of the present invention 5;
Fig. 6 is the shear viscosity of oil-filled solution polymerized butadiene styrene rubber 2550 and the log-log graph of shear rate of the LG chemistry of the embodiment of the present invention 6.
Embodiment
The present invention relates to a kind of detection method of tyre rubber processing characteristics, the detecting step of described method is as follows:
(1) mooney's viscosimeter is adopted to carry out Mooney viscosity test to rubber sample; Described rubber sample is selected from the product of the different batches that the different supplier of rubber of the same race or same provider provide; Described rubber sample is at least 50 groups;
(2), after the rubber sample of the same race cutting to the Mooney viscosity value tested out in step (1) close (the described close interval value referring to standard value ± 3), torque rheometer is put into;
Torque rheometer inputs the rate of specific gravity of rubber sample, weighs and extrude quality, the numerical value of record shear viscosity and shear stress under each speed, according to the numerical value of shear rate and apparent shear viscosity, simulate the power-law equation of rubber sample;
Described power-law equation is as follows:
lgη＝(A±0.03)lgγ+(B±0.06)
In formula, η is apparent shear viscosity, and γ is shear rate, and A is n-1, and described n is non-newtonian index, and B is LgK, the apparent viscosity that described K is shear rate when being 0;
(3) meet the power-law equation of the described rubber sample of step (2), then the rheological property of described tyre rubber is qualified; Do not meet the power-law equation of the described rubber sample of step (2), then the rheological property of described tyre rubber is defective.
As one embodiment of the present of invention, described torque rheometer is Single screw extrusion, capillary die; The wherein use of following parameter, for the detection method of tyre rubber processing characteristics of the present invention accuracy be important, concrete: the specification of capillary die is L/D=10, L/D=20, L/D=30, L/D=40, the rotating speed of extrusion screw rod is 1r/min ~ 30r/min, extrusion temperature is 110 DEG C ~ 170 DEG C, and each rate of extrusion lower retention time is 60s.The present invention adopts torque rheometer kapillary to extrude pattern can measure different temperatures, the shear stress under different shear rate and apparent shear viscosity, by arranging the rotating speed of screw rod and the kapillary using different length-diameter ratio, can reach 0 ~ 500S
-1shear rate, the scope of the shear rate of mixer mixing and extrusion process can be contained, according to great many of experiments, draw not same material power-law equation and coefficient range, the processing stability energy of Accurate Prediction rubber in actual production.
As one embodiment of the present of invention, described rubber sample is natural rubber or synthetic rubber; Described synthetic rubber is butadiene rubber, styrene-butadiene rubber, ethylene-propylene-diene rubber or butyl rubber.Preferably, described styrene-butadiene rubber is solution polymerized butadiene styrene rubber or emulsion polymerized styrene butadiene rubber; Preferably, described solution polymerized butadiene styrene rubber is non-oil-filled solution polymerized butadiene styrene rubber or oil-filled solution polymerized butadiene styrene rubber, and described emulsion polymerized styrene butadiene rubber is non-oil-filled emulsion polymerized styrene butadiene rubber or oil-filled emulsion polymerized styrene butadiene rubber.
Tyre rubber is typical polymkeric substance, along with the increase of shear rate, the apparent viscosity of polymkeric substance reduces, this phenomenon is called " shear shinning " behavior (shear-thinning), usually claims pseudoplastic fluid (pseudoplasticfluid) the fluid with " shear shinning " effect.The flowing law of pseudoplastic fluid meets Ostwald-deWale power-law equation (powerlaw):
After taking the logarithm in both sides:
lgη＝lgK+(n-1)lgγ
Wherein η is apparent shear viscosity, and γ is shear rate, and A is n-1, and wherein n is non-newtonian index, and B is LgK, and the apparent viscosity that wherein K is shear rate when being 0, is called viscosity constant.
By carrying out rheology testing to rubber not of the same race, draw corresponding shear rate and apparent viscosity value, after double-log is got to the two, the corresponding power-law equation of matching; Fitting result shows the different manufacturers that Mooney viscosity is close, fabrication process condition is identical, the rubber of the same race of different batches meets power-law equation lg η=(A ± 0.03) lg γ+(B ± 0.06), and the rubber meeting this equation in use processing characteristics is stablized; Do not meet the material of the party's journey, need the adjustment carrying out working process parameter according to actual conditions in advance.Namely adopt torque rheometer kapillary extrusion method to detect the close rubber material of Mooney viscosity value, predict the processing characteristics of this kind of material in actual production.
The different batches of rubber not of the same race or rubber of the same race all has different A values and B value, but rubber material of the same race has certain A value and B value, the rubber material for all: A value scope is standard value ± 0.03, and the scope of B value is standard value ± 0.06.
The test of described crude rubber Mooney viscosity is with reference to GB/T1232.1 standard, and adopt disk to shear viscosity meter and measure, the principle of measurement is: at 100 DEG C, preheating 1min, and heating 4min, rotor speed is the torque value under 2r/min condition, i.e. the variable of Mooney viscosity.
Described employing torque rheometer kapillary is extruded pattern and is extruded tire rubber, torque rheometer temperature is raised to the temperature value pre-set, according to different glue kind, screw rod and extrusion neck ring mold temperature 110 DEG C ~ 170 DEG C are set, rate of extrusion program and time are set, according to the extent of reaction of rubber kind to temperature and shearing force, screw speed is set, guarantee that shear rate contains actual production medium shear rate scope, after equipment for the treatment of is thermally-stabilised in advance, rubber to be measured is cut into slice, test from high length-diameter ratio (L/D=40) capillary die, the quality of sample extruded in record, the numerical value of shear viscosity and pressure.
This method of testing adopts torque rheometer to test, and this equipment can be applied to rubber compounding simultaneously, and tire half parts extrusion die is intended, and has wide range of applications, and all refers to that between guide-car, actual processing uses.
In order to the elastomeric processing characteristics of more deep understanding, Mooney viscosity value only by detecting rubber can not the usability of complete reflection material, capillary rheometer can carry out the comparison of polymkeric substance different structure, similar polymers is due to molecular chain structure difference, as linear, side chain length, block structure etc., be reflected in difference capillary rheometer just showing as shear stress and apparent viscosity.
As one embodiment of the present of invention, described torque rheometer is mixing type torque rheometer, is a kind of multi-functional interchangeable brick pattern torque detection instrument, comprises small size closed mixer, small-sized screw extruder and dissimilar extrusion neck ring mold.The extrusion neck ring mold that the present invention uses is slit capillary die, and namely torque rheometer kapillary extrudes pattern, can the actual process of analog synthesis rubber, characterizes elastomeric processing rheological property.
List the power-law equation embodiment of concrete rubber material below, so that the present invention is described further, but protection scope of the present invention is not limited in this:
Embodiment 1:
Get the non-oil-filled emulsion polymerized styrene butadiene rubber 1502 of bright and beautiful lake petrochemical industry, mooney's viscosimeter is adopted to measure the Mooney viscosity value (ML1+4100 DEG C) of rubber, then rubber sample is cut into strip, at torque rheometer Single screw extrusion, test under the pattern of capillary die, the specification of capillary die is L/D=20, L/D=30, L/D=40, screw rod is set and extrusion neck ring mold temperature is 150 DEG C, the rate of extrusion of singe screw is 1r/min, 5r/min, 10r/min, 15r/min, 20r/min, 25r/min, 30r/min, and each rate of extrusion lower retention time is 60s, the rate of specific gravity of input rubber, weigh and extrude quality under each speed, the numerical value of record shear stress and shear viscosity, according to the numerical value of shear viscosity and shear rate, show that the power-law equation of this material is as table 1.Figure 1 shows that the non-oil-filled shear viscosity of emulsion polymerized styrene butadiene rubber 1502 and the log-log graph of shear rate of the bright and beautiful lake petrochemical industry of the embodiment of the present invention 1.
Embodiment 2:
Get the non-oil-filled emulsion polymerized styrene butadiene rubber 1502 of Qilu Petrochemical, mooney's viscosimeter is adopted to measure the Mooney viscosity value (ML1+4100 DEG C) of rubber, then rubber sample is cut into strip, at torque rheometer Single screw extrusion, test under the pattern of capillary die, the specification of capillary die is L/D=20, L/D=30, L/D=40, screw rod is set and extrusion neck ring mold temperature is 150 DEG C, the rate of extrusion of singe screw is 1r/min, 5r/min, 10r/min, 15r/min, 20r/min, 25r/min, 30r/min, and each rate of extrusion lower retention time is 60s, the rate of specific gravity of input rubber, weigh and extrude quality under each speed, draw the numerical value of shear stress and shear viscosity, according to the numerical value of apparent shear viscosity and shear rate, show that elastomeric power-law equation is as table 1.Figure 2 shows that the non-oil-filled shear viscosity of emulsion polymerized styrene butadiene rubber 1502 and the log-log graph of shear rate of the Qilu Petrochemical of the embodiment of the present invention 2.
Embodiment 3:
Get the non-oil-filled emulsion polymerized styrene butadiene rubber 1502 raising sub-petrochemical industry, mooney's viscosimeter is adopted to measure the Mooney viscosity value (ML1+4100 DEG C) of rubber, then rubber sample is cut into strip, at torque rheometer Single screw extrusion, test under the pattern of capillary die, the specification of capillary die is L/D=20, L/D=30, L/D=40, screw rod is set and extrusion neck ring mold temperature is 150 DEG C, the rate of extrusion of singe screw is 1r/min, 5r/min, 10r/min, 15r/min, 20r/min, 25r/min, 30r/min, and each rate of extrusion lower retention time is 60s, the rate of specific gravity of input rubber, weigh and extrude quality under each speed, the numerical value of record shear stress and shear viscosity, according to the numerical value of apparent shear viscosity and shear rate, show that the power-law equation of this material is as table 1.Figure 3 shows that the non-oil-filled shear viscosity of emulsion polymerized styrene butadiene rubber 1502 of raising sub-petrochemical industry and the log-log graph of shear rate of the embodiment of the present invention 3.
Embodiment 4:
Get the non-oil-filled emulsion polymerized styrene butadiene rubber 1500E of Jilin Petrochemical, mooney's viscosimeter is adopted to measure the Mooney viscosity value (ML1+4100 DEG C) of rubber, then rubber sample is cut into strip, at torque rheometer Single screw extrusion, test under the pattern of capillary die, the specification of capillary die is L/D=20, L/D=30, L/D=40, screw rod is set and extrusion neck ring mold temperature is 150 DEG C, the rate of extrusion of singe screw is 1r/min, 5r/min, 10r/min, 15r/min, 20r/min, 25r/min, 30r/min, and each rate of extrusion lower retention time is 60s, the rate of specific gravity of input rubber, weigh and extrude quality under each speed, the numerical value of record shear stress and shear viscosity, according to the numerical value of apparent shear viscosity and shear rate, show that the power-law equation of this material is as table 1.Figure 4 shows that the non-oil-filled shear viscosity of emulsion polymerized styrene butadiene rubber 1502 and the log-log graph of shear rate of the Jilin Petrochemical of the embodiment of the present invention 4.
Embodiment 5:
Get the oil-filled solution polymerized butadiene styrene rubber 6270M of bright and beautiful lake petrochemical industry, mooney's viscosimeter is adopted to measure the Mooney viscosity value (ML1+4100 DEG C) of rubber, then rubber sample is cut into strip, at torque rheometer Single screw extrusion, test under the pattern of capillary die, the specification of capillary die is L/D=20, L/D=30, L/D=40, screw rod is set and extrusion neck ring mold temperature is 150 DEG C, the rate of extrusion of singe screw is 1r/min, 5r/min, 10r/min, 15r/min, 20r/min, 25r/min, 30r/min, and each rate of extrusion lower retention time is 60s, the rate of specific gravity of input rubber, weigh and extrude quality under each speed, the numerical value of record shear stress and shear viscosity, according to the numerical value of apparent shear viscosity and shear rate, show that the power-law equation of this material is as table 1.Figure 5 shows that the oil-filled shear viscosity of solution polymerized butadiene styrene rubber 6270M and the log-log graph of shear rate of the bright and beautiful lake petrochemical industry of the embodiment of the present invention 5.
Embodiment 6:
Get the oil-filled solution polymerized butadiene styrene rubber 2550 of LG chemistry, mooney's viscosimeter is adopted to measure the Mooney viscosity value (ML1+4100 DEG C) of rubber, then rubber sample is cut into strip, at torque rheometer Single screw extrusion, test under the pattern of capillary die, the specification of capillary die is L/D=20, L/D=30, L/D=40, screw rod is set and extrusion neck ring mold temperature is 150 DEG C, the rate of extrusion of singe screw is 1r/min, 5r/min, 10r/min, 15r/min, 20r/min, 25r/min, 30r/min, and each rate of extrusion lower retention time is 60s, the rate of specific gravity of input rubber, weigh and extrude quality under each speed, the numerical value of record shear stress and shear viscosity, according to the numerical value of apparent shear viscosity and shear rate, show that the power-law equation of this material is as table 1.Figure 6 shows that the shear viscosity of oil-filled solution polymerized butadiene styrene rubber 2550 and the log-log graph of shear rate of the LG chemistry of the embodiment of the present invention 6.
The Mooney viscosity of the styrene-butadiene rubber of table 1 different manufacturers and power-law equation contrast table
As can be seen from Table 1, the Mooney viscosity value difference of the SBR1502 (containing 1500E) of four producers in embodiment 1-embodiment 4 is within 5%, and in the use procedure of workshop, do not carry out the adjustment of process conditions, after kapillary extrusion test, draw shear rate and the apparent viscosity value of polymer melt, after getting double-log, draw lg η=(n-1) lg γ+LgK, wherein n-1=A ± 0.03, LgK=B ± 0.06, after detecting the different manufacturers SBR1502 shear rate that draws and apparent viscosity value, draw A=-0.61, B=4.68.
The Mooney viscosity difference of embodiment 5 and embodiment 6 folding two kinds of oil-filled solution polymerized butadiene styrene rubbers is also within 5%, meet the oil-filled solution polymerized butadiene styrene rubber (butadiene content 23.5% of workshop steady production, oil-filled for 37.5phr) power-law equation be lg η=(-0.80 ± 0.03) lg γ+(4.83 ± 0.06), the power-law equation of example 5 and example 6 is within the scope of described power-law equation.
In the present invention, the process need of concrete the Fitting Calculation applies to Matlab or similar functions software, utilizes least square method to determine to differ minimum fitted data with actual value.
The present invention can summarize with other the concrete form without prejudice to spirit of the present invention or principal character.Therefore, no matter from which point, above-mentioned embodiment of the present invention all can only be thought explanation of the present invention and can not limit the present invention, claims indicate scope of the present invention, and scope of the present invention is not pointed out in above-mentioned explanation, therefore, any change in the implication suitable with claims of the present invention and scope, all should think to be included in the scope of claims of the present invention.
Claims (5)
1. a detection method for tyre rubber processing characteristics, is characterized in that, the detecting step of described method is as follows:
(1) mooney's viscosimeter is adopted to carry out Mooney viscosity test to rubber sample;
(2) to after the close rubber sample of the same race cutting of the Mooney viscosity value tested out in step (1), torque rheometer is put into; Torque rheometer inputs the rate of specific gravity of rubber sample, weighs and extrude quality, the numerical value of record shear viscosity and shear stress under each speed, according to the numerical value of shear rate and apparent shear viscosity, simulate the power-law equation of rubber sample;
Described power-law equation is as follows:
lgη＝(A±0.03)lgγ+(B±0.06)
In formula, η is apparent shear viscosity, and γ is shear rate, and A is n-1, and described n is non-newtonian index, and B is LgK, the apparent viscosity that described K is shear rate when being 0;
(3) meet the power-law equation of the described rubber sample of step (2), then the rheological property of described tyre rubber is qualified; Do not meet the power-law equation of the described rubber sample of step (2), then the rheological property of described tyre rubber is defective.
2. the detection method of tyre rubber processing characteristics as claimed in claim 1, it is characterized in that, described torque rheometer is Single screw extrusion, capillary die, the specification of capillary die is L/D=10, L/D=20, L/D=30, L/D=40, the rotating speed of extrusion screw rod is 1r/min ~ 30r/min, extrusion temperature is 110 DEG C ~ 170 DEG C, and each rate of extrusion lower retention time is 60s.
3. the detection method of tyre rubber processing characteristics as claimed in claim 1 or 2, it is characterized in that, described rubber sample is natural rubber or synthetic rubber; Described synthetic rubber is butadiene rubber, styrene-butadiene rubber, ethylene-propylene-diene rubber or butyl rubber.
4. the detection method of tyre rubber processing characteristics as claimed in claim 3, it is characterized in that, described styrene-butadiene rubber is solution polymerized butadiene styrene rubber or emulsion polymerized styrene butadiene rubber; Described solution polymerized butadiene styrene rubber is non-oil-filled solution polymerized butadiene styrene rubber or oil-filled solution polymerized butadiene styrene rubber, and described emulsion polymerized styrene butadiene rubber is non-oil-filled emulsion polymerized styrene butadiene rubber or oil-filled emulsion polymerized styrene butadiene rubber.
5. the detection method of tyre rubber processing characteristics as claimed in claim 1 or 2, it is characterized in that, described torque rheometer is mixing type torque rheometer.
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| CN108262217A (en) * | 2016-12-30 | 2018-07-10 | 财团法人工业技术研究院 | Method and system for coating non-Newtonian fluid material |
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| US6412337B1 (en) * | 2000-01-28 | 2002-07-02 | Polyvalor S.E.C. | Apparatus and method for measuring the rheological properties of a power law fluid |
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| CN108262217A (en) * | 2016-12-30 | 2018-07-10 | 财团法人工业技术研究院 | Method and system for coating non-Newtonian fluid material |
| CN108262217B (en) * | 2016-12-30 | 2020-01-03 | 财团法人工业技术研究院 | Method and system for coating non-Newtonian fluid material |
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