KR20200055587A - Analysis method for insoluble sulphur based material and method for manufacturing tire - Google Patents

Abstract

Embodiments of the present invention provide a method for analyzing an insoluble sulfur-based material which improves accuracy and stability, and accordingly, provide a method for manufacturing a tire which can improve process efficiency and produce a high-quality tire. One embodiment of the present invention discloses a method for analyzing an insoluble sulfur-based material, which comprises: a material preparation step of preparing a sample material containing insoluble sulfur; a heat measurement step of measuring the heat change amount of the sample material containing the insoluble sulfur while heating the sample material containing the insoluble sulfur; a graph preparation step of comprising generating a graph of the heat change amount of the sample material containing the insoluble sulfur by using data measured in the heat measurement step; and a conversion amount analysis step of measuring the soluble sulfur conversion amount of the sample material containing the insoluble sulfur by calculating an area for each region in the graph generated in the graph preparation step.

Description

{Analysis method for insoluble sulphur based material and method for manufacturing tire}

Embodiments of the present invention relates to an insoluble sulfur-based material analysis method and a tire manufacturing method.

Sulfur is used in a variety of fields, for example, alone or in combination with other materials and used in various industrial products.

As a specific example, sulfur is used for tire production using rubber, and as a specific example, it is mixed with a rubber composition to facilitate molding of the tire.

In order to improve the manufacturing characteristics of the tire, it may be necessary to precisely control the process, especially in a process in which heat is applied.

However, it is not easy to measure the thermal stability of the material containing sulfur, and it is dangerous to the human body and has limitations in improving accuracy.

Embodiments of the present invention provide a method for analyzing an insoluble sulfur-based material that improves accuracy and stability, thereby providing a tire manufacturing method capable of improving the process efficiency and manufacturing a high-quality tire.

In one embodiment of the present invention, a material preparation step of preparing a sample material containing insoluble sulfur, and a heat measurement step of measuring a heat change amount of the sample material containing insoluble sulfur while heating the sample material containing insoluble sulfur , Graph preparation step comprising generating a graph of the amount of heat change of the sample material containing the insoluble sulfur using the data measured in the thermal measurement step, and calculating the area of each area in the graph generated in the graph preparation step Thus, an insoluble sulfur-based material analysis method including a conversion amount analysis step of measuring a soluble sulfur conversion amount of a sample containing the insoluble sulfur is disclosed.

In this embodiment, the thermal measurement step may include heating the sample material from 30 to 50 degrees Celsius to 240 to 270 degrees Celsius.

In the present embodiment, the conversion amount analysis step may include a step of dividing a region in the graph and comparing an area of all or a portion of each divided region.

Another embodiment of the present invention is a material preparation step of preparing a sample material containing insoluble sulfur, and a heat measurement step of measuring a heat change amount of the sample material containing insoluble sulfur while heating the sample material containing insoluble sulfur. , Graph preparation step comprising generating a graph of the amount of heat change of the sample material containing the insoluble sulfur using the data measured in the thermal measurement step, calculates the area for each area in the graph generated in the graph preparation step Insoluble sulfur to determine the thermal stability of the insoluble sulfur sample by comparing the result of the analysis through the conversion amount analysis step and the conversion amount analysis step to measure the amount of soluble sulfur conversion of the sample containing the insoluble sulfur by setting conditions Disclosed is a tire manufacturing method comprising a sample determination step.

In this embodiment, through the step of determining the insoluble sulfur sample may include the step of mixing the insoluble sulfur material that meets the set conditions in the rubber composition and then proceeding to the rolling process.

Other aspects, features, and advantages other than those described above will become apparent from the following drawings, claims, and detailed description of the invention.

The insoluble sulfur-based material analysis method according to the present embodiment can accurately and safely grasp the thermal stability characteristics of the insoluble sulfur, thereby providing a tire manufacturing method that improves process efficiency and manufactures high-quality tires. Can be.

1 is a flowchart illustrating a method for analyzing an insoluble sulfur-based material according to an embodiment of the present invention.
FIG. 2 is a schematic view of an apparatus used in the method for analyzing the insoluble material based on the insoluble bow of FIG. 1.
3 and 4 are views for explaining the method for analyzing the insoluble sulfur-based material of FIG. 1.
5 and 6 are views showing a tire manufacturing method according to an embodiment of the present invention and tires manufactured through the tire manufacturing method.

The present invention can be applied to various transformations and may have various embodiments, and specific embodiments will be illustrated in the drawings and described in detail in the detailed description. Effects and features of the present invention and methods for achieving them will be clarified with reference to embodiments described below in detail with reference to the drawings. However, the present invention is not limited to the embodiments disclosed below, but may be implemented in various forms.

Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings, and the same or corresponding components will be denoted by the same reference numerals, and redundant description thereof will be omitted. .

In the following examples, terms such as first and second are not used in a limited sense, but for the purpose of distinguishing one component from other components.

In the following embodiments, the singular expression includes the plural expression unless the context clearly indicates otherwise.

In the examples below, terms such as include or have are meant to mean the presence of features or components described in the specification, and do not preclude the possibility of adding one or more other features or components in advance.

In the drawings, the size of components may be exaggerated or reduced for convenience of description. For example, since the size and thickness of each component shown in the drawings are arbitrarily shown for convenience of description, the present invention is not necessarily limited to what is shown.

In the following embodiments, the x-axis, y-axis, and z-axis are not limited to three axes on the Cartesian coordinate system, and can be interpreted in a broad sense including them. For example, the x-axis, y-axis, and z-axis may be orthogonal to each other, but may refer to different directions that are not orthogonal to each other.

When an embodiment can be implemented differently, a specific process order may be performed differently from the described order. For example, two processes described in succession may be performed substantially simultaneously, or may be performed in an order opposite to that described.

1 is a flow chart illustrating a method for analyzing an insoluble sulfur-based material according to an embodiment of the present invention, and FIG. 2 is a diagram schematically showing an apparatus used in the method for analyzing an insoluble material based on insoluble bow.

3 and 4 are views for explaining the method for analyzing the insoluble sulfur-based material of FIG. 1.

The insoluble sulfur-based material analysis method of this embodiment can be applied in various ways. For example, it may be used in fields using materials containing sulfur. As a specific example, insoluble sulfur may be contained in a rubber composition material for manufacturing a tire, and properties of the insoluble sulfur material contained in the material for manufacturing such a tire may be examined, and whether or not the insoluble sulfur material is used may be determined in advance. have.

Referring first to Figure 1, the insoluble sulfur-based material analysis method may include a material preparation step (S10), a thermal measurement step (S20), a graph preparation step (S30), and a conversion amount analysis step (S40).

The material preparation step S10 may include preparing a sample material containing insoluble sulfur.

Insoluble sulfur can be used for a variety of applications. For example, an insoluble sulfur may be mixed with a rubber composition for manufacturing a tire to prepare a compounded rubber, and the compounded rubber may be manufactured through a high temperature process such as rolling to produce a tire.

The process for manufacturing such a tire, for example, a rolling process, is a high-temperature equipment process, and the thermal stability of the material is very important, and thus, thermal stability of the material containing sulfur may be required.

Insoluble sulfur may be mixed in rubber materials for the tire rolling process because the occurrence of defects in the process is not high in an expensive or thermal process, and the insoluble sulfur may have a phase in accordance with time or an increase in heating temperature during a high temperature heating process. It may be necessary to analyze the thermal properties of insoluble sulfur through sampling prior to tire manufacture as it changes and thus turns to soluble sulfur.

The sample material containing insoluble sulfur may include preparing a material containing 90% or more of insoluble sulfur. For example, it may include preparing a sample containing at least 95 percent, more specifically at least 98 percent insoluble sulfur.

The thermal measurement step (S20) may include measuring the amount of heat change of the sample material containing the insoluble sulfur while heating the sample material containing the insoluble sulfur prepared in the material preparation step (S10).

This step may be performed using a variety of methods, for example, may include heating the sample material for a period of time in a temperature range.

As a specific example, the method may include heating the sample at 20 to 40 degrees Celsius per minute (min), and for example, starting from 30 to 50 degrees Celsius and 240 to 270 degrees Celsius for a sample material containing insoluble sulfur. Heating to a degree.

In the process of heating the sample material containing the insoluble sulfur, there is a temperature change in the sample material, and this temperature change may indicate exothermic or endothermic properties of the sample material, through which changes in the phase of the material containing the insoluble sulfur And the amount of conversion to soluble sulfur.

As an optional embodiment, the step of measuring the amount of heating and heat change may use the device (DSU) of FIG. 2.

The device DSU may include a sample unit SM, a reference unit RU, a heating unit HM, a sensing unit SS, and a control unit CU.

The sample unit SM includes an area in which a sample material containing the insoluble sulfur can be disposed, and as an optional embodiment, may have a crucible shape to facilitate heating through the heating unit HM.

The reference unit RU may be arranged independently of the sample unit SM, and may be arranged to be heated using a heating unit HM, and as an optional embodiment, may be arranged for the reference material It includes a region, and may have a crucible shape to facilitate heating through the heating unit HM as an optional embodiment. In addition, as an optional embodiment, the sample unit SM and the reference unit RU may be independently heated. For example, a unit for the sample unit SM and a unit for the reference unit RU may be separately provided in the heating unit HM.

The heating unit HM may perform a heating process using various methods. For example, a heating process may be performed using a current.

The sensing unit SS may be formed to sense each of the sample unit RU and the reference unit RU, and specifically detect a change in temperature. In addition, the energy supply through the heating unit HM during the heating process for the sample unit RU and the reference unit RU, for example, the amount of change in current can be measured.

The control unit CU may grasp the amount of heat change of the insoluble sample material through the sensing unit SS.

For example, when there is a temperature change for the sample material of the sample unit SM during the heating process through the heating unit HM, the sample is sampled through the heating unit HM so that it becomes equal to the temperature of the reference material of the reference unit RU. It is possible to control the current supplied to the unit SM and the reference unit RU.

For example, when the sample material material of the sample unit SM melts and the temperature changes as the phase transition occurs, thereby detecting a temperature difference with the reference unit RU, heating through the heating unit HM to compensate for this. It can measure the amount of current supplied.

For example, during the heating process between the sample unit SM and the reference unit RU, a temperature difference occurs due to a phase change according to a property of the material, and a signal of a current supplied to compensate for the temperature difference is controlled by the controller CU ) And use this to know the heat flow of the sample material of the sample unit SM. As a specific example, the characteristics of heat generation or heat absorption can be seen.

As an optional embodiment, such a device (DSU) may include a differential scanning calorimeter (DSC).

The graph preparation step S30 may include generating a graph of the amount of heat change of the sample material containing the insoluble sulfur using the data measured in the thermal measurement step S20.

The graph may include various forms, for example, may be a measure of the amount of heat change according to the change in temperature.

Specifically, the X-axis may represent a temperature, and this temperature may be a temperature for heating the sample material. Also, the X-axis may represent time, and may indicate the time for heating the sample material.

The Y-axis may represent heat flow. For example, the Y-axis may represent Q / T, that is, the amount of heat flow per unit time.

Referring to Figure 3 illustratively shows a graph generated in the graph preparation step (S30).

As an optional embodiment, FIG. 3 may show heat flow while the heating process is performed for a sample material from 40 degrees Celsius to 250 degrees Celsius.

Referring to Figure 3, depending on the temperature, t1, t2, t3 and t4 in the heat flow (heat flow) changes, this point may indicate that endothermic. These temperatures t1, t2, t3 and t4 are defined as the first, second, third, and fourth heat flow change temperature points.

For example, four convex upwards may be continuous, and the temperature at each apex of these four convex lines may represent t1, t2, t3 and t4.

In addition, it is possible to determine the temperature at which the heat flow begins to change and the temperature at which the heat flow changes based on the first, second, third, and fourth heat flow change temperature points t1, t2, t3, and t4. It may be a temperature range in which the state of the sample material, including turmeric, changes. For example, the starting point T1 and the ending point T2 of the heat flow change can be obtained based on the first heat flow change temperature point t1.

Using this, the change start temperature T1, the boundary temperature T2, the boundary temperature T3, the boundary temperature T4, and the change end temperature T5 can be obtained.

For example, the change start temperature T1, the boundary temperature T2, the boundary temperature T3, the boundary temperature T4, and the change end temperature T5 can be obtained using t1, t2, t3, and t4. As a specific example, assuming that t1, t2, t3, and t4 correspond to values similar to the intermediate values of change start temperature T1, boundary temperature T2, boundary temperature T3, boundary temperature T4, and change end temperature T5, change start temperature T1, boundary temperature T2, boundary temperature T3, boundary temperature T4, and change end temperature T5 can be obtained.

In addition, as another example, a change start temperature T1, a boundary temperature T2, a boundary temperature T3, a boundary temperature T4, and a change end temperature T5 can be obtained by using the temperature at a point corresponding to inflection points on the graph. For example, the lowest point of the valley between the curve representing the vertex of t1 and the curve representing the curve of t2 can be defined as T2.

As an optional embodiment, these divalent methods, i.e., t1, t2, t3 and t4, and a method using an inflection point of the curve are mixed to change the starting temperature T1, boundary temperature T2, boundary temperature T3, boundary temperature T4 and The end temperature of change T5 can be determined.

As an optional embodiment, t1 may be 93 degrees Celsius to 97 degrees Celsius, specifically 95 degrees Celsius, t2 may be 111 degrees Celsius to 115 degrees Celsius, and specifically, 113 degrees Celsius, t3 may be 123 degrees Celsius to 127 degrees Celsius, specifically For example, it may be 125 degrees Celsius, and t4 may be 135 degrees Celsius to 139 degrees Celsius, and specifically, 137 degrees Celsius.

As an optional embodiment, T1 may be 83 degrees to 87 degrees Celsius, specifically 85 degrees Celsius, T2 may be 103 degrees to 107 degrees Celsius, specifically 105 degrees Celsius, and T3 may be 118 degrees to 122 degrees Celsius, specifically For example, it may be 122 degrees Celsius, T4 may be 128 degrees to 132 degrees Celsius, specifically 130 degrees Celsius, and T5 may be 143 degrees to 147 degrees Celsius, and specifically 145 degrees Celsius.

The conversion amount analysis step (S40) may include a conversion amount analysis step of calculating the area of each area in the graph generated in the graph preparation step (S30) to measure the amount of soluble sulfur conversion of the sample containing the insoluble sulfur. .

Referring to FIG. 3, the graph may be divided into four spaces by a change start temperature T1, a boundary temperature T2, a boundary temperature T3, a boundary temperature T4, and a change end temperature T5.

Each space may be defined as a first state area (Sa), a second state area (Sb), a third state space (Sc), and a fourth state space (Sd).

In addition, the first state region (Sa), the second state region (Sb), the third state space (Sc) and the fourth state space (Sd) region of the insoluble sulfur sample material changes the state of the phase (phase) It can be defined as a different area.

For example, the first state region Sa is sulfur (alpha), the second state region Sb is sulfur (beta), the third state space Sc is sulfur (lambda), and the fourth state space Sd is It can be defined as representing Hwang (mu).

And, the sulfur (alpha) of the first state region Sa is soluble sulfur, the sulfur (beta) of the second state region Sb is soluble sulfur, and the sulfur (lambda) of the third state space Sc is insoluble sulfur And sulfur (mu) in the fourth state space (Sd) may be defined as representing insoluble sulfur.

In addition, the areas of the first state region Sa, the second state region Sb, the third state space Sc, and the fourth state space Sd may be proportional to the amount of heat flow and proportional to the amount of phase change. Therefore, the ratio of insoluble sulfur to soluble sulfur can be obtained using this area.

That is, if the area of the first state region Sa and the area of the second state region Sb are added, it can be said to be proportional to the sum of soluble sulfur, and the area of the third state space Sc and the fourth state space Sd It can be said that adding the area of is proportional to the sum of insoluble sulfur.

To this end, the area of the first state area Sa, the area of the second state area Sb, the area of the third state space Sc, and the area of the fourth state space Sd can be obtained, respectively. For example, it can be obtained using an integral method.

As an optional embodiment, as shown in FIG. 4, a method of obtaining an area of a graph having a predetermined reference point or more, a partial area of the first state area Sa, a partial area of the second state area Sb, and a third state space Sc The partial area of and the partial area of the fourth state space Sd may be obtained.

For example, draw a connecting line segment connecting two points where T1 and T2, which are the boundaries of the first state area Sa, of the first state area Sa and the graph meet, and obtain the area of the graph above the connecting line segment It can be defined as a partial area of the first state region Sa.

In addition, draw a connecting line segment connecting two points where T2 and T3, which are the boundaries of the second state area Sb, of the second state area Sb and the graph meet, and obtain the area of the graph above the connecting line segment to obtain the second area. It can be defined as a partial area of the state region Sb.

Also, draw a connecting line segment connecting the two points where the graph meets T3 and T4, which are the boundaries of the third state area Sc, among the third state areas Sc, and obtain the area of the graph on the connecting line segment to obtain the third It can be defined as a partial area of the state region Sc.

In addition, a connecting line segment connecting two points where the graph meets T4 and T5, which are the boundaries of the fourth state area Sd, of the fourth state area Sd is drawn, and the area of the graph on the connecting line segment is obtained to obtain the fourth It can be defined as a partial area of the state area Sd.

As illustrated in FIG. 4, the partial area of the first state area Sa, the partial area of the second state area Sb, the partial area of the third state space Sc, and the part of the fourth state space Sd It is possible to know the phase change state of a more precise insoluble sulfur sample material by using a lot of actual heat flow changes using the area.

The partial area of the first state region Sa obtained by this method is F (Sa), the partial area of the second state region Sb is F (Sb), and the partial area of the third state space Sc is F (Sc) ) And the partial area of the fourth state space Sd may be defined as F (Sd).

Through these results, it is possible to analyze how much of the insoluble sulfur sample material was converted to soluble sulfur during the heating process for the insoluble sulfur sample material.

For example, in the heating process for the insoluble sulfur sample material, the amount of the insoluble sulfur sample material changed to soluble sulfur is proportional to the sum of F (Sa) and F (Sb), and the remaining amount of insoluble sulfur sample is F (Sc) and F It can be defined as being proportional to the sum of (Sd).

As a specific example, F (Sa), F (Sb), F (Sc), and F (Sd) may be 50%, 35%, 10%, and 5%, respectively, based on 100. That is, in this case, it can be defined that soluble sulfur is 85% and insoluble sulfur remains 15%.

Through this method, it is possible to infer the amount of conversion of the insoluble sulfur sample material to soluble sulfur during the heating process, and the analogy method may be similar to or more accurate than other methods, for example, an analytical method using toxic toluene. .

The insoluble sulfur-based material analysis method of the present embodiment may include a material preparation step, a thermal measurement step, a graph preparation step, and a conversion amount analysis step.

It may include the step of preparing a sample material containing insoluble sulfur, and measuring the amount of heat change while proceeding with the heating process. For example, heat flow can be measured. As a specific example, it can be measured using a DSC device. You can then use these results to create a graph.

By generating such a graph, it is possible to easily grasp the degree of conversion of the soluble sulfur according to the temperature of the insoluble sulfur sample material using the area on the graph.

Through this, it is possible to analyze the insoluble sulfur-based material, and specifically, it is possible to easily grasp characteristics of thermal stability.

As an example, an insoluble sulfur may be contained in a rubber composition material for manufacturing a tire, and characteristics of the insoluble sulfur material contained in the material for manufacturing such a tire may be examined, and whether or not the insoluble sulfur material is used may be determined in advance. have.

That is, sulfur may be added during tire production using a rubber composition, and insoluble sulfur may be included in consideration of thermal stability. Meanwhile, the tire may be manufactured through a rolling process at a high temperature with respect to the rubber composition containing such insoluble sulfur.

On the other hand, in this high temperature process, insoluble sulfur can be converted to soluble sulfur after a certain time, so it is necessary to grasp the thermal stability characteristics of insoluble sulfur in advance.

Using the method of this embodiment, a sample of an insoluble sulfur material may be collected in advance before mixing into the rubber composition, and then thermal properties thereof may be easily grasped. As a specific example, it is possible to grasp the thermal characteristics while heating at a constant temperature, for example, heating from 40 degrees Celsius to 250 degrees Celsius, and also at a heating rate of 20 to 40 degrees Celsius per minute (min), and after heating, insoluble sulfur and soluble sulfur The amount of can be known, and accordingly, it is easy to grasp how much insoluble sulfur is converted to soluble sulfur.

As an optional embodiment, the amount of the insoluble sulfur converted to soluble sulfur is compared to a set condition, for example, 85 percent, and a value greater than this, specifically 90 percent, is determined to be an insoluble sulfur material that does not meet the thermal stability condition. can do.

As a result, it is possible to easily grasp the thermal stability characteristics for the insoluble sulfur material. In addition, this method is harmless to the human body and can reduce environmental pollution when compared to a method using a harmful material for human body, for example, toluene.

5 and 6 are views showing a tire manufacturing method according to an embodiment of the present invention and tires manufactured through the tire manufacturing method.

5, the tire 100 is shown.

Referring to the tire 100, the tread portion 110 and the side wall 180 may be included. For example, the tire 100 may be manufactured using the tire manufacturing method of this embodiment.

The tire 100 may have a shape extending in the circumferential direction RT about the central axis AX. In addition, the tire 100 may be coupled to a rim (not shown) on the inner side based on the radial direction r from the central axis AX.

The tread unit 110 may include an area facing the road surface when driving after the tire 100 is mounted on the vehicle. For example, the tread unit 110 may include an area in contact with the road surface when the vehicle is running.

The tread portion 110 may have one or more patterns, and a plurality of grooves may be formed adjacent to the patterns.

The side wall 180 is connected to the tread part 110. A bead part (not shown) for stably coupling the tire 100 with a rim (not shown) may be disposed in an area opposite to the area connected to the tread part 110 among the areas of the sidewall 180.

The bead portion (not shown) may have various shapes, for example, may have a rectangular or hexagonal wire bundle-shaped region coated with rubber on a steel wire, through which the tire 100 is It can be seated and secured to the rim. In addition, the bead portion (not shown) may be provided with a cushioning region that distributes the load on the wire bundle-shaped region and reduces external impact.

Referring to FIG. 6, the tire manufacturing method includes a material preparation step (S110), a thermal measurement step (S120), a graph preparation step (S130), a conversion amount analysis step (S140), and an insoluble sulfur sample determination step (S150) and a manufacturing process step. It may include (S160).

The material preparation step (S110) may include preparing a sample material containing insoluble sulfur.

Insoluble sulfur can be used for a variety of applications. For example, an insoluble sulfur may be mixed with a rubber composition for manufacturing a tire to prepare a compounded rubber, and the compounded rubber may be manufactured through a high temperature process such as rolling to produce a tire.

The process for manufacturing such a tire, for example, a rolling process, is a high-temperature equipment process, and the thermal stability of the material is very important, and thus, thermal stability of the material containing sulfur may be required.

Insoluble sulfur may be mixed in rubber materials for the tire rolling process because the occurrence of defects in the process is not high in an expensive or thermal process, and the insoluble sulfur may have a phase in accordance with time or an increase in heating temperature during a high temperature heating process. It may be necessary to analyze the thermal properties of insoluble sulfur through sampling prior to tire manufacture as it changes and thus turns to soluble sulfur.

The sample material containing insoluble sulfur may include preparing a material containing 90% or more of insoluble sulfur. For example, it may include preparing a sample containing at least 95 percent, more specifically at least 98 percent insoluble sulfur.

The thermal measurement step (S120) may include measuring a heat change amount of the sample material containing the insoluble sulfur while heating the sample material containing the insoluble sulfur prepared in the material preparation step (S110).

The thermal measurement step (S120) is the same as described in the above-described embodiment or may be selectively modified and applied, so a detailed description thereof will be omitted.

In addition, the device DSU of FIG. 2 described above may be used in this step.

The graph preparation step S130 may include generating a graph of the amount of heat change of the sample material containing the insoluble sulfur using the data measured in the thermal measurement step S120.

The graph may include various forms, for example, may be a measure of the amount of heat change according to the change in temperature.

Specifically, the X-axis may represent a temperature, and this temperature may be a temperature for heating the sample material. Also, the X-axis may represent time, and may indicate the time for heating the sample material.

The Y-axis may represent heat flow. For example, the Y-axis may represent Q / T, that is, the amount of heat flow per unit time.

Graph preparation step (S130) is the same as described in the above-described embodiment, or may be selectively modified and applied, so a detailed description thereof will be omitted.

For example, the graphs of FIGS. 3 and 4 and an analysis method therefor may be used as they are.

In addition, the above description of t1, t2, t3, and t4 and the numerical ranges thereof can be applied as it is.

In addition, the above description of T1, T2, T3, T4, T5 and the numerical ranges thereof can be applied as it is.

Conversion amount analysis step (S140) may include a conversion amount analysis step of calculating the area of each area in the graph generated in the graph preparation step (S130) to measure the amount of soluble sulfur conversion of the sample containing the insoluble sulfur. .

This can be applied by modifying the same or similar to that described in the above-described embodiment, so a detailed description is omitted.

For example, it can be divided into four spaces by T1, T2, T3, T4, and T5 of the graph of FIG. 3 described above, and each space is a first state area (S1a), a second state area (S1b), and a first It is defined as the three-state space S1c and the fourth-state space S1d, and the area of these regions can be used.

For example, the first state area S1a is sulfur (alpha), the second state area S1b is sulfur (beta), the third state space S1c is sulfur (lambda), and the fourth state space S1d is It can be defined as representing Hwang (mu).

In addition, sulfur (alpha) in the first state region S1a is soluble sulfur, sulfur (beta) in the second state region S1b is soluble sulfur, and sulfur (lambda) in the third state space S1c is insoluble sulfur And sulfur (mu) in the fourth state space S1d may be defined as representing insoluble sulfur.

Also, the areas of the first state region S1a, the second state region S1b, the third state space S1c, and the fourth state space S1d may be proportional to the amount of heat flow and proportional to the amount of phase change. Therefore, the ratio of insoluble sulfur to soluble sulfur can be obtained using this area.

That is, adding the area of the first state region S1a and the area of the second state region S1b is proportional to the sum of soluble sulfur, and the area of the third state space S1c and the fourth state space S1d It can be said that adding the area of is proportional to the sum of insoluble sulfur.

The contents of the method for obtaining the area of each region are the same as those described in the above-described embodiment, and thus detailed contents are omitted.

The partial area of the first state area S1a obtained in this way is F (S1a), the partial area of the second state area S1b is F (S1b), and the partial area of the third state space S1c is F (S1c) ) And the partial area of the fourth state space S1d can be defined as F (S1d), and it can be analyzed how much of the insoluble sulfur sample material was converted to soluble sulfur during the heating process for the insoluble sulfur sample material.

For example, in the heating process for the insoluble sulfur sample material, the amount of the insoluble sulfur sample material changed to soluble sulfur is proportional to the sum of F (S1a) and F (S1b), and the remaining amount of the insoluble sulfur sample is F (S1c) and F It can be defined as being proportional to the sum of (S1d).

As a specific example, F (S1a), F (S1b), F (S1c), and F (S1d) may be 50%, 35%, 10%, and 5%, respectively, based on 100. That is, in this case, it can be defined that soluble sulfur is 85% and insoluble sulfur remains 15%.

Through this method, it is possible to infer the amount of conversion of the insoluble sulfur sample material to soluble sulfur during the heating process, and the analogy method may be similar to or more accurate than other methods, for example, an analytical method using toxic toluene. .

In the step of determining the insoluble sulfur sample (S150), the above value, that is, after the heating process for the insoluble sulfur sample material, may include comparing the amount of insoluble sulfur or soluble sulfur with a set condition.

For example, the set condition may have an amount of soluble sulfur as a value, and a specific example may have a value of 85 percent.

In this case, the insoluble sulfur sample material is a value measured through the above method after the heating process for the insoluble sulfur sample material, that is, when the amount of the soluble sulfur exceeds 85 percent, specifically, when it has a value of 90 percent, the insoluble sulfur sample material is It can be understood that the thermal stability is not better than the insoluble sulfur determined as the setting condition.

As another example, when the amount of soluble sulfur is 85 percent, it can be understood that the above insoluble sulfur sample material is a material that meets the set conditions of thermal stability.

In the manufacturing process step (S160), a tire manufacturing process may be performed using a rubber composition containing insoluble sulfur.

For example, as a result of the determination of the insoluble sulfur sample in the determination step (S150), after mixing the insoluble sulfur material in the rubber composition when the thermal stability satisfies the set condition, the process of rolling the compounded rubber is performed. Then, further processing steps can be performed to manufacture the tire.

Through this, it is possible to reduce or prevent process troubles during a high temperature rolling process using a rubber composition, thereby improving tire manufacturing efficiency and improving the quality of the manufactured tire.

The tire manufacturing method of this embodiment may use an insoluble sulfur-based material analysis method. Specifically, it may include a material preparation step, a thermal measurement step, a graph preparation step, a conversion amount analysis step, an insoluble sulfur sample determination step, and a manufacturing process step.

It may include the step of preparing a sample material containing insoluble sulfur, and measuring the amount of heat change while proceeding with the heating process. For example, heat flow can be measured. As a specific example, it can be measured using a DSC device. You can then use these results to create a graph.

By generating such a graph, it is possible to easily grasp the degree of conversion of the soluble sulfur according to the temperature of the insoluble sulfur sample material using the area on the graph.

Through this, it is possible to analyze the insoluble sulfur-based material, and specifically, it is possible to easily grasp characteristics of thermal stability.

Insoluble sulfur may be contained in the rubber composition material for manufacturing a tire, and the properties of the insoluble sulfur material contained in the material for manufacturing such a tire may be examined, and it may be determined in advance whether or not the insoluble sulfur material is used.

That is, sulfur may be added during tire production using a rubber composition, and insoluble sulfur may be included in consideration of thermal stability. On the other hand, it is possible to manufacture a tire through a rolling process at a high temperature with respect to a rubber casting containing such insoluble sulfur.

On the other hand, in this high temperature process, insoluble sulfur can be converted to soluble sulfur after a certain time, so it is necessary to grasp the thermal stability characteristics of insoluble sulfur in advance.

Using the method of this embodiment, a sample of an insoluble sulfur material may be collected in advance before mixing into the rubber composition, and then thermal properties thereof may be easily grasped. As a specific example, it is possible to grasp the thermal characteristics while heating at a constant temperature, for example, heating from 40 degrees Celsius to 250 degrees Celsius, and also at a heating rate of 20 to 40 degrees Celsius per minute (min), and after heating, insoluble sulfur and soluble sulfur The amount of can be known, and accordingly, it is easy to grasp how much insoluble sulfur is converted to soluble sulfur.

As an optional embodiment, the amount of the insoluble sulfur converted to soluble sulfur is compared to a set condition, for example, 85 percent, and a value greater than this, specifically 90 percent, is determined to be an insoluble sulfur material that does not meet the thermal stability condition. can do.

As a result, it is possible to easily grasp the thermal stability characteristics for the insoluble sulfur material. In addition, this method is harmless to the human body and can reduce environmental pollution when compared to a method using a harmful material for human body, for example, toluene.

Using this, it is possible to easily measure the thermal stability of the insoluble sulfur mixed with the rubber composition, and determine whether to select the insoluble sulfur material from which the corresponding sample is taken. In addition, the specific ratio of the insoluble sulfur of the soluble sulfur to the insoluble sulfur material in addition to the thermal stability can also be known for the insoluble sulfur material that satisfies the setting conditions of the thermal stability, and more specifically, the ratio of each phase of sulfur. For example sulfur in the first state, eg sulfur (alpha), sulfur in the second state, eg sulfur (beta), sulfur in the third state, eg sulfur (lambda) and sulfur in the fourth state , For example, since the ratio of the amount of conversion and residual amount depending on the heat of sulfur (mu) can be known, heating conditions during heating such as a rolling process for a rubber composition containing an insoluble sulfur material, specifically, for heating temperature and heating rate Precise control can be facilitated.

Through the precise handling of the insoluble sulfur, the tire manufacturing process can be smoothly performed, and the efficiency can be improved to reduce the defective tire manufacturing rate during manufacturing. In addition, it is possible to improve the quality of the tire after all the manufacturing processes.

As described above, the present invention has been described with reference to the embodiments shown in the drawings, but these are merely exemplary, and those skilled in the art will understand that various modifications and equivalent other embodiments are possible therefrom. . Therefore, the true technical protection scope of the present invention should be determined by the technical spirit of the appended claims.

The specific implementations described in the embodiments are exemplary embodiments, and do not limit the scope of the embodiments in any way. In addition, unless specifically mentioned, such as "essential", "important", etc., it may not be a necessary component for the application of the present invention.

In the specification (especially in the claims) of an embodiment, the use of the term "above" and similar indication terms may be in both singular and plural. In addition, when the range is described in the embodiment As it includes the invention to which the individual values belonging to the above range are applied (if there is no contrary description), it is the same as describing each individual value constituting the above range in the detailed description. Finally, the method for constructing the method according to the embodiment Unless explicitly stated or contrary to the steps, the steps may be performed in an appropriate order. The embodiments are not necessarily limited to the order of description of the steps. In the embodiments, all examples or exemplary terms ( The use of, for example, “etc.” is merely for describing the embodiment in detail, and the scope of the embodiment is not limited by the examples or exemplary terms, unless it is limited by the claims. In addition, those skilled in the art can recognize that various modifications, combinations, and changes can be configured according to design conditions and factors within the scope of the appended claims or equivalents thereof.

S10, S110: material preparation steps
S20, S120: Thermal measurement step
S30, S130: graph preparation steps
S40, S140: Conversion amount analysis step
S150: insoluble sulfur sample determination step
S160: Manufacturing process steps

Claims (5)

A material preparation step of preparing a sample material containing insoluble sulfur;
A thermal measurement step of measuring a heat change amount of the sample material containing the insoluble sulfur while heating the sample material containing the insoluble sulfur;
A graph preparation step comprising generating a graph of the amount of heat change of the sample material containing the insoluble sulfur using the data measured in the thermal measurement step; And
Insoluble sulfur-based material analysis method comprising a conversion amount analysis step of calculating the area of each area in the graph generated in the graph preparation step to measure the amount of soluble sulfur conversion of the sample containing the insoluble sulfur. According to claim 1,
The thermal measurement step comprises the step of heating from 30 to 50 degrees Celsius to 240 to 270 degrees Celsius with respect to the sample material insoluble sulfur-based material analysis method. According to claim 1,
The conversion amount analysis step comprises the step of partitioning the regions in the graph, and comparing the area of all or part of each partitioned region. A material preparation step of preparing a sample material containing insoluble sulfur;
A thermal measurement step of measuring a heat change amount of the sample material containing the insoluble sulfur while heating the sample material containing the insoluble sulfur;
A graph preparation step comprising generating a graph of the amount of heat change of the sample material containing the insoluble sulfur using the data measured in the thermal measurement step;
A conversion amount analysis step of calculating an area for each region in the graph generated in the graph preparation step to measure a soluble sulfur conversion amount of the sample containing the insoluble sulfur; And
A tire manufacturing method comprising a step of determining an insoluble sulfur sample to determine the thermal stability of the insoluble sulfur sample by comparing the result analyzed through the conversion amount analysis step with a set condition. According to claim 4,
The tire manufacturing method comprising the step of mixing the insoluble sulfur material that meets the set conditions through the determination of the insoluble sulfur sample to the rubber composition and then proceeding with a rolling process.

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