KR20220109205A - A method for evaluate abrasion of resin composition - Google Patents

Abstract

The present invention provides an abrasion evaluation method of a resin composition, which can measure an abrasion degree according to a type, a size, and a mixing ratio of a filler inside a resin composition and can predict an effect where the resin composition including the filler can affect processing equipment, in advance. The method comprises a step of compressing the resin composition existing on a pad by a rotation compression means.

Description

A method for evaluating abrasion of a resin composition {A method for evaluate abrasion of resin composition}

The present application relates to a method for evaluating abrasion of a resin composition.

The resin composition may include a filler in order to secure heat dissipation (thermal conductivity) or to secure thixotropy as required in the process.

For example, as the treatment of heat generated in batteries such as electric products, electronic products, or secondary batteries in recent years has become an important issue, a resin composition in which a filler is mixed with a resin component is used.

Patent Document 1 is known for a battery module to which such a resin composition is applied. In order to inject the resin composition into such a battery module, an injection device or the like is used. At this time, since the resin composition contains a filler and the hardness of the filler is generally high, there is a problem in that the injection device is worn.

In consideration of the wear problem of the injection device, etc., a filler of low hardness was used or the content of the filler was lowered, but the desired heat dissipation or thixotropic properties of the resin composition could not be secured.

In this situation, there is a need for a method for evaluating abrasion of a resin composition that objectively and accurately predicts the degree of wear applied by the equipment used in the actual process when manufacturing a resin composition containing a filler due to the resin composition.

Republic of Korea Patent Publication No. 10-2016-0105354

The present application provides a method for evaluating abrasion of a resin composition.

In addition, the present application provides a method for evaluating abrasion of a resin composition capable of measuring abrasion according to the type, size, and mixing ratio of the filler of the resin composition.

In addition, the present application provides a method for evaluating abrasion of a resin composition for objectively and accurately predicting the degree of wear applied by the equipment used in the actual process when manufacturing a resin composition containing a filler due to the resin composition.

Among the physical properties mentioned in the present application, when the measured temperature affects the physical properties, unless otherwise specified, the corresponding physical properties are those measured at room temperature.

The term room temperature as used in the present application is a natural temperature that is not heated or cooled, and for example, any one temperature within the range of 10°C to 30°C, may be a temperature of about 23°C or about 25°C.

The wear evaluation method according to an example of the present application may include pressing the resin composition present on the pad with a rotary pressing means.

In addition, the wear evaluation method according to an example of the present application is suitable for measuring the abrasion of a resin composition including a resin composition and a resin component, including a resin component and a filler, by measuring the abrasion level of the resin composition.

In the wear evaluation method according to an example of the present application, the resin composition may be present on a polishing pad. The resin composition may be present by being loaded onto the pad. In this case, the pad may provide a space in which the resin composition, which is the measurement target of the abrasion, is placed.

The pad preferably withstands the rotation and pressurization environment performed while measuring the abrasion of the resin composition. At this time, the specific rotation and pressurization environment will be described below. In addition, the pad may have an appropriate frictional force so that the resin composition loaded on the surface does not come off and does not affect the abrasion of the wear specimen, and the surface thereof is not very hard or soft and has appropriate hardness. can

Although the characteristics that the pad can have are listed as described above, if the pad has a surface characteristic that does not affect the abrasion of the wear specimen in a series of processes of the abrasion evaluation method without the resin composition loaded on the surface of the pad being separated It is not particularly limited.

For the pad, MD-nap, MD-Dur, MD-Dac, MD-mol, MD-plan, MD-plusm, MD-Chem, MD-Pan, MD-Floc, or MD-Sat, which are products of STRUERS, can be used. This is not particularly limited.

When measuring abrasion in the wear evaluation method according to an example of the present application, in order to prevent the pad from being fixed by the rotation and pressure environment, thereby affecting the wear of the wear specimen, the pad is made of a resin A magnet member may be provided on a surface opposite to the surface on which the composition is present.

The shape of the pad is not particularly limited, and may be, for example, a rectangle or a circle. In addition, the width of the pad is not particularly limited, and while providing a space in which the resin composition is appropriately placed, it is sufficient that the resin composition is not separated to the outside of the pad when measuring abrasion.

In the wear evaluation method according to an example of the present application, the rotational pressing means may include a pressure plate on which a wear specimen is mounted. For example, the pressure plate may be provided with a space for mounting a wear specimen, and may be used by mounting the wear specimen in the space. In addition, the space is not particularly limited in shape and may be, for example, a square or a circle. If the pressure plate can also form the space, the shape is not particularly limited, and may be, for example, a square or a circle.

The rotation pressing means may rotate about a rotation axis. In addition, the distance between the axis of rotation of the rotating pressing means and the center of the wear specimen mounted on the pressing plate may be 40 mm or more, 42 mm or more, 44 mm or more, or 46 mm or more, and in another example, 60 mm or less, 57.5 mm or less, 55 mm or less, 52.5 mm or less, 50 mm or less, or 47.5 mm or less. Here, the center of the wear specimen may be the center of gravity.

When the distance between the rotational axis of the rotational pressing means and the center of the wear specimen mounted on the pressing plate satisfies the above range, the resin composition present in the pad is not biased and can be in contact with the wear specimen evenly, so it is possible to evaluate the wear effectively .

The resin composition may be in contact with the wear specimen. The wear specimen is abrasion generated by the resin composition, and refers to a specimen for measuring the abrasion level of the resin composition.

The shape of the wear specimen is not particularly limited, but may be selected according to the shape of the space provided in the pressure plate. In addition, there are cases where a toric shape is used as a fastener for injection equipment used in the manufacturing process of the resin composition, and the wear specimen may have a toric shape considering that the abrasion of the resin composition should occur well. .

When the wear specimen is a toric body, the ratio of the outer diameter to the inner diameter of the wear specimen may be 1.25 or more, 1.5 or more, or 1.75 or more, and in another example, 5 or less, 4 or less, 3 or less, or 2.5 or less.

When the ratio of the inner diameter and the outer diameter of the wear specimen, which is a toric body, satisfies the above range, it is possible to measure abrasion with high accuracy. When the ratio of inner diameter and outer diameter is smaller than the above range, the contact area between the resin composition and the wear specimen is reduced, and the measurement efficiency is lowered. may be destroyed.

In addition, the outer diameter of the toroidal wear specimen may be 25 mm or more, 28 mm or more, 30 mm or more, or 32 mm or more, and in another example, 40 mm or less, 38 mm or less, or 36 mm or less. In addition, when the wear specimen is toric, the thickness of the wear specimen may be 0.5 mm or more, 0.75 mm or more, 1 mm or more, 1.25 mm or more, 1.5 mm or more, or 1.75 mm or more, and in another example, 3 mm or less, 2.8 mm or less, 2.6 mm or less, 2.4 mm or less, or 2.2 mm or less.

On the other hand, the wear specimen may have a Brinell hardness (KS B 0805) of about 175 HB or more, 177.5 HB or more, 180 HB or more, 182.5 HB or more, or 185 HB or more, and in another example, 195 HB or less, 192.5 HB or more or less or 190 HB or less. When the Brinell hardness of the wear specimen satisfies the above range, it is suitable for evaluating the abrasion of the resin composition including the resin component and the filler.

The type of the wear specimen is not particularly limited, but as the wear specimen, stainless steel may be included in order to prevent effects such as corrosion from requirements other than the resin composition.

The wear specimen may be in contact with the resin composition. The wear specimen mounted on the pressing plate may be rotated by rotating the rotation pressing means, and at this time, the wear specimen in contact with the resin composition continuously generates friction with the resin composition. Here, the surface of the wear specimen continuously rubbed by the resin composition is abraded while being polished.

The rotation pressing means may be rotated by an external force, and the rotational speed may be maintained within the range of about 30 rpm or more, 35 rpm or more, 40 rpm or more, or 45 rpm or more, and in another example, 60 rpm or less, 57.5 rpm or less, It may be maintained within the range of 55 rpm or less or 52.5 rpm or less. When the rotation speed of the wear specimen satisfies the above range, it is possible to prevent the resin composition from leaving the pad. The rotation pressing means may rotate about a rotation axis, and the rotation axis may form an angle within the range of 0 degrees to 10 degrees with the direction of the pressing.

The resin composition may be pressed by means of a rotary pressing means. When pressurized, the frictional force on the contact surface between the wear specimen and the resin composition increases, enabling efficient wear measurement.

The wear specimen may transmit the external force to the resin composition. That is, the wear specimen may transmit rotational force and pressure to the resin composition while in contact with the resin composition.

At this time, the pressurization may be performed at a pressure of 15 N or less, 14 N or less, 13 N or less, 12 N or less, or 11 N or less. In addition, the lower limit of the pressurization is not particularly limited unless it is 0 N, but it is sufficient that the wear specimen and the resin composition can be more closely adhered.

When the pressure satisfies the above range, it is possible to prevent the resin composition from escaping to the outside of the pad.

In addition, the pressurization may be 3 minutes or more, 4 minutes or more, 5 minutes or more, 6 minutes or more, 7 minutes or more, 8 minutes or more, or 9 minutes or more, and the resin composition is suitably worn to evaluate the degree of wear. it is not

The rotary pressing means may press the resin composition present on the pad. In this case, the direction of pressing may form an angle within the range of 0 degrees to 10 degrees with the normal of the pad surface.

The wear degree evaluation method of the resin composition according to an example of the present application may evaluate the abrasion degree according to Equation 1 below. Here, the degree of wear of the resin composition may mean an absolute value of ΔW (unit: %) calculated according to Equation 1 below.

[Formula 1]

△W = (W _f -W _i )/W _i ×100

In Equation 1, W _f is the mass (unit: g) of the wear specimen after finishing pressing, and W _i is the mass (unit: g) of the wear specimen before pressing.

By measuring the amount of wear of the wear specimen, the degree of wear of the resin composition can be measured.

The method for evaluating abrasion of a resin composition according to an example of the present application includes selecting a resin composition having an absolute value of abrasion ΔW of 0.45% or less, 0.44% or less, 0.43% or less, 0.42% or less, 0.41% or less, or 0.4% or less. can be additionally performed.

In addition, the method for evaluating abrasion of the resin composition according to an example of the present application may be a method for selecting a resin composition or a method for preparing a resin composition as described above. Here, in the case of the manufacturing method of the resin composition, the step of mixing the resin component and the filler so that the absolute value of the wear degree ΔW is 0.45% or less may be performed.

The resin composition may include a resin component and a filler. In addition, the resin component includes not only a component generally known as a resin, but also a component that can be converted into a resin through a curing reaction or a polymerization reaction. In addition, the resin composition includes not only a component generally known as a resin, but also a component that can be converted into a resin through a curing reaction or a polymerization reaction.

The resin component as a term used in the present application includes not only a component generally known as a resin, but also a component that can be converted into a resin through a curing reaction or a polymerization reaction. In one example, as the resin component, an adhesive resin or a precursor capable of forming an adhesive resin may be applied. Examples of such a resin component include an acrylic resin, an epoxy resin, a urethane resin, an olefin resin, an ethylene vinyl acetate (EVA) resin, or a silicone resin, or a precursor such as a polyol or an isocyanate compound, but this It is not limited.

Here, the polyol refers to a compound containing two or more hydroxyl groups, and may be referred to as a diol if it contains two hydroxyl groups and a triol if it contains three hydroxyl groups. In addition, the isocyanate compound means a compound containing one or more isocyanate groups, and when it contains two isocyanate groups, it may be called a diisocyanate compound. That is, the resin component may include diol or diisocyanate.

In addition, the resin composition may be an adhesive composition, that is, an adhesive by itself, or a composition capable of forming an adhesive through a reaction such as a curing reaction. Such a resin composition may be a solvent-type resin composition, a water-based resin composition, or a solvent-free resin composition.

In addition, the resin composition may be a one-component resin composition or a two-component resin composition. The two-component resin composition is separated into a main composition and a curing agent composition as is known, and a resin can be formed by mixing and reacting the two separated compositions. The resin composition including the resin component and the filler may refer to the main composition, the curing agent composition, a mixture thereof, or a state after the reaction after mixing them.

Also, the resin composition may be a urethane resin composition or a two-component urethane resin composition. The two-component urethane resin composition is a composition capable of forming a resin by mixing the main composition and the curing agent composition, and in this case, the polyurethane may be formed by the reaction of the main agent and the curing agent.

In addition, the resin composition is, in one example, the main composition of the two-component urethane resin composition, the curing agent composition of the two-component urethane resin composition, or a mixture of the main and curing agent composition, or the urethane resin is formed by the urethane reaction in the mixture. may refer to mixtures.

In the two-component urethane resin composition, the main composition of a polyol may include a polyol, and the curing agent composition may include an isocyanate compound such as polyisocyanate.

In addition, the resin composition may include a filler in order to ensure thermal conductivity of the cured product thereof.

The term thermal conductivity of the present application refers to the ASTM D5470 standard or ISO 22007 along the thickness direction of the sample in a state in which the resin composition is prepared as a disk-type sample (hardened product) having a diameter of 2 cm or more and a thickness of 500 μm. -2 When measured according to the standard, it may mean a case of showing thermal conductivity of about 1.5 W/m·K or more.

In another example, the thermal conductivity is 1.5 W/m·K or more, 1.6 W/m·K or more, 1.7 W/m·K or more, 1.8 W/m·K or more, 1.9 W/m·K or more, 2.0 W/ m K or more, 2.1 W/m K or more, 2.2 W/m K or more, 2.3 W/m K or more, 2.4 W/m K or more, 2.5 W/m K or more, 2.6 W/m K or more It may be about K or more, 2.7 W/m·K or more, 2.8 W/m·K or more, 2.9 W/m·K or more, or 3.0 W/m·K or more. Since the higher the thermal conductivity, the higher the thermal conductivity, the upper limit thereof is not particularly limited. For example, the thermal conductivity is 20 W/m·K or less, 18 W/m·K or less, 16 W/m·K or less, 14 W/m·K or less, 12 W/m·K or less, 10 W /m·K or less, 8 W/m·K or less, 6 W/m·K or less, or 4 W/m·K or less.

The form or content ratio of the filler is not particularly limited. For example, in consideration of the viscosity of the resin composition, the possibility of precipitation of the filler in the resin composition, desired thermal resistance or thermal conductivity, insulation, filling effect or dispersibility, etc., spherical and plate-like shapes may be selected, and the content The ratio may also be appropriately adjusted.

In addition, if insulating properties can be secured, application of a carbon filler such as graphite may be considered. For example, the carbon filler may use activated carbon.

The shape of the filler may be appropriately selected and used in a spherical and/or non-spherical shape (eg, needle-shaped and plate-shaped, etc.) as needed, but is not limited thereto.

As a filler, 1 type(s) or 2 or more types suitably selected as needed can be used. In addition, even if the same type of filler is used, different shapes may be mixed and used, or those having different average particle diameters may be mixed and used. For example, aluminum hydroxide and aluminum oxide may be mixed and used as a filler, and their shapes and average particle diameters may be different from each other.

In general, the smaller the size of the filler, the higher the viscosity of the resin composition and the higher the possibility that the filler settles in the cured product of the resin composition. Moreover, there exists a tendency for thermal resistance to become high, so that the size of a filler becomes large. Therefore, an appropriate type of filler may be selected in consideration of the above points, and if necessary, two or more types of fillers may be used.

In addition, it is advantageous to use a spherical filler in consideration of the amount to be filled, but a filler having a shape such as a needle-shaped or plate-shaped filler may also be used in consideration of thermal conductivity.

In one example, the resin composition may include a filler having an average particle diameter in the range of 0.001 μm to 80 μm. In another example, the average particle diameter of the filler may be 80 μm or less, 76 μm or less, 72 μm or less, 68 μm or less, or 64 μm or less, and in another example, the average particle diameter is 40 μm or more, 44 μm or more, 48 μm or more, 52 It may be greater than or equal to 56 µm or greater than or equal to 56 µm. In addition, in another example, the average particle diameter of the filler may be less than 40 μm, 36 μm or less, 32 μm or less, or 28 μm or less, and in another example, the average particle diameter may be 5 μm or more, 7.5 μm or more, 10 μm or more, or 12.5 μm or more. have. In another example, the average particle diameter of the filler may be less than 5 μm, 4 μm or less, 3 μm or less, or 1 μm or less, and in another example, the average particle diameter is 0.001 μm or more, 0.01 μm or more, 0.05 μm or more, 0.1 μm or more, 0.2 μm or more, 0.4 μm or more, 0.8 μm or more, or 1 μm or more.

In this case, the average particle diameter of the filler is a so-called D50 particle diameter (median particle diameter), and may mean a particle diameter at 50% cumulative by volume of the particle size distribution. That is, the particle size distribution is obtained on the basis of the volume, and the average particle diameter can be viewed as the particle diameter at the point where the cumulative value is 50% on the cumulative curve with the total volume being 100%. The D50 particle size as described above may be measured by a laser diffraction method.

In this case, the filler content ratio and/or particle size ratio may be adjusted in consideration of the resin and combination to be mixed together.

The self thermal conductivity of the filler may be at least about 1 W/m·K, at least about 5 W/m·K, at least about 10 W/m·K, or at least about 15 W/m·K, in another example about 400 W /m·K or less, about 350 W/m·K or less, or about 300 W/m·K or less.

If the filler has thermal conductivity within the above range, the type thereof is not particularly limited, but may include inorganic particles in consideration of availability and compatibility with the resin component.

The inorganic particles include, for example, oxides such as aluminum oxide, magnesium oxide, beryllium oxide or titanium oxide; nitrides such as boron nitride, silicon nitride or aluminum nitride, and carbides such as silicon carbide; hydrated metals such as aluminum hydroxide or magnesium hydroxide; metal fillers such as copper, silver, iron, aluminum or nickel; It may be a metal alloy filler such as titanium, but is not limited thereto.

Considering the resin included in the resin composition and ultimately securing the desired thermal conductivity, inorganic particles having a Mohs hardness of about 6 or more are generally selected. However, inorganic particles having a Mohs hardness of 6 or more have advantageous properties in terms of heat conduction, but may cause damage to equipment due to their high surface hardness. Therefore, in order to prevent such a problem, the filler may further include inorganic particles having a Mohs hardness of less than 6.

Inorganic particles having a Mohs hardness of less than 6 have disadvantageous properties compared to inorganic particles having a Mohs hardness of 6 or more in terms of thermal conductivity. can

The inorganic particles having a Mohs hardness of 6 or more include, for example, aluminum oxide (alumina) and the like, and are not particularly limited. The inorganic particles having a Mohs hardness of less than 6 include, for example, aluminum hydroxide and the like, and are not particularly limited.

In addition, the inorganic particles having a Mohs hardness of 6 or more may have a Mohs hardness of 7 or more, 8 or more, or 9 or more, and the inorganic particles having a Mohs hardness of 6 or less may have a Mohs hardness of 5 or less, 4 or less, or 3 or less.

Fillers can include spherical and non-spherical particles. In the present application, the term spherical particle means a particle having a sphericity of about 0.95 or more, and a non-spherical particle means a particle having a sphericity of less than 0.95.

The sphericity can be confirmed through particle shape analysis. Specifically, the sphericity of the filler, which is a three-dimensional particle, may be defined as a ratio (S'/S) of the surface area (S) of the particle to the surface area (S') of a sphere having the same volume of the particle. For real particles, we usually use circularity. The circularity is obtained by obtaining a two-dimensional image of an actual particle and expressed as a ratio of the boundary P of the image and the boundary of a circle having the same area (A) as the image, and is obtained by the following equation.

<Circularity formula>

Circularity=4πA/P ²

The circularity is expressed as a value from 0 to 1, a perfect circle has a value of 1, and irregularly shaped particles have a value lower than 1. The sphericity value in this specification was taken as the average value of the circularity measured with Marvern's vertical analysis equipment (FPIA-3000).

The present application may provide a method for evaluating abrasion of a resin composition capable of measuring abrasion according to the type, size, and mixing ratio of fillers in the resin composition.

In addition, the present application may provide a method for evaluating abrasion of a resin composition that can predict in advance the effect that a resin composition containing a filler may have on process equipment by measuring the abrasion of the resin composition.

1 is a diagram schematically illustrating an apparatus including a pad and a rotation pressing means according to an example of the present application.
2 is a diagram schematically illustrating a surface of a pressure plate according to an example of the present application.

Hereinafter, the present invention will be described with reference to Examples and Comparative Examples, but the scope of the present invention is not limited by the contents presented below.

<Method of measuring physical properties>

1. Measuring method of average particle diameter of filler (D50 particle diameter)

The average particle diameter of the filler is the D50 particle diameter, also called the so-called median particle diameter, and is the particle diameter (median diameter) at 50% cumulative of the volume-based cumulative curve of the particle size distribution. Such a particle size may be defined as a particle diameter at a point where the cumulative value becomes 50% on a cumulative curve in which the particle size distribution is calculated on a volume basis and the total volume is 100%. The D50 particle size can be measured using the MASTERSIZER 3000 equipment of Marven in accordance with ISO-13320, and ethanol was used as the solvent.

2. Method for evaluating the sphericity of fillers

The sphericity of a filler may be defined as a ratio (S'/S) of a surface area (S) of a particle to a surface area (S') of a sphere having the same volume of the particle. For real particles, we usually use circularity. The circularity is obtained by obtaining a two-dimensional image of an actual particle and expressed as a ratio of the boundary P of the image and the boundary of a circle having the same area (A) as the image, and is obtained by the following equation.

<Circularity formula>

Circularity=4πA/P ²

The circularity is expressed as a value from 0 to 1, a perfect circle has a value of 1, and irregularly shaped particles have a value lower than 1. The sphericity value in this specification was taken as the average value of the circularity measured with Marvern's vertical analysis equipment (FPIA-3000).

<Preparation of resin composition>

Preparation Example 1

As a resin component, a diol compound (A, weight average molecular weight (M _w ): 400 g/mol) was mixed with the filler (B) in a weight ratio of 100:1,000 (A:B) to prepare a resin composition.

As the filler (B), a mixture of three types of fillers having different average particle diameters (D50 particle diameter) was applied. Specifically, spherical alumina (B1) having an average particle diameter (D50 particle diameter) of about 70 μm, spherical alumina (B2) having an average particle diameter (D50 particle diameter) of about 20 μm, and average particle diameter (D50 particle diameter) of about 2 μm A filler in which phosphorus non-spherical alumina (B3) was mixed in a weight ratio of 6:2:2 (B1:B2:B3) was used.

In the above, the spherical alumina is an alumina having a sphericity of 0.95 or more, and the non-spherical alumina is an alumina having a sphericity of less than 0.95. Hereinafter, the definition of spherical alumina or non-spherical alumina is as described above.

Preparation 2

Spherical alumina (B1) having an average particle diameter (D50 particle diameter) of about 70 μm, non-spherical alumina (B2) having an average particle diameter (D50 particle diameter) of about 10 μm, and ratio having an average particle diameter (D50 particle diameter) of about 2 μm A resin composition was prepared in the same manner as in Preparation Example 1, except that a filler mixed with spherical alumina (B3) in a weight ratio of 6:2:2 (B1:B2:B3) was used.

Preparation 3

Spherical alumina (B1) having an average particle diameter (D50 particle diameter) of about 70 μm, non-spherical alumina (B2) having an average particle diameter (D50 particle diameter) of about 10 μm, and ratio having an average particle diameter (D50 particle diameter) of about 2 μm A resin composition was prepared in the same manner as in Preparation Example 1, except that a filler mixed with spherical alumina (B3) in a weight ratio of 5:2:3 (B1:B2:B3) was used.

Preparation 4

Spherical alumina (B11) with an average particle diameter (D50 particle diameter) of about 70 μm, aluminum hydroxide (B12) with an average particle diameter (D50 particle diameter) of about 65 μm, and non-spherical shape with an average particle diameter (D50 particle diameter) of about 20 μm A filler obtained by mixing alumina (B2) and non-spherical alumina (B3) having an average particle diameter (D50 particle diameter) of about 2 μm in a weight ratio of 4:2:2:2 (B11:B12:B2:B3) is used Except that, a resin composition was prepared in the same manner as in Preparation Example 1.

Preparation 5

Spherical alumina (B11) with an average particle diameter (D50 particle diameter) of about 70 μm, non-spherical alumina (B13) with an average particle diameter (D50 particle diameter) of about 60 μm, and ratio with an average particle diameter (D50 particle diameter) of about 20 μm Using a filler mixed with spherical alumina (B2) and non-spherical alumina (B3) having an average particle diameter (D50 particle diameter) of about 2 μm in a weight ratio of 4:2:2:2 (B11:B13:B2:B3) Except for that, a resin composition was prepared in the same manner as in Preparation Example 1.

Preparation 6

Spherical alumina (B11) with an average particle diameter (D50 particle diameter) of about 70 μm, aluminum hydroxide (B12) with an average particle diameter (D50 particle diameter) of about 65 μm, and non-spherical shape with an average particle diameter (D50 particle diameter) of about 10 μm A filler obtained by mixing alumina (B2) and non-spherical alumina (B3) having an average particle diameter (D50 particle diameter) of about 2 μm in a weight ratio of 4:2:2:2 (B11:B12:B2:B3) is used Except that, a resin composition was prepared in the same manner as in Preparation Example 1.

Preparation 7

Spherical alumina (B11) with an average particle diameter (D50 particle diameter) of about 70 μm, aluminum hydroxide (B12) with an average particle diameter (D50 particle diameter) of about 60 μm, and non-spherical shape with an average particle diameter (D50 particle diameter) of about 65 μm Alumina (B13), non-spherical alumina (B2) having an average particle diameter (D50 particle diameter) of about 10 μm, and non-spherical alumina (B3) having an average particle diameter (D50 particle diameter) of about 2 μm were mixed 2:2:2:2 A resin composition was prepared in the same manner as in Preparation Example 1, except that a filler mixed in a weight ratio of :2 (B11:B12:B13:B2:B3) was used.

Preparation 8

Spherical alumina (B1) having an average particle diameter (D50 particle diameter) of about 40 μm, non-spherical alumina (B2) having an average particle diameter (D50 particle diameter) of about 10 μm, and ratio having an average particle diameter (D50 particle diameter) of about 2 μm A resin composition was prepared in the same manner as in Preparation Example 1, except that a filler mixed with spherical alumina (B3) in a weight ratio of 4:3:3 (B1:B2:B3) was used.

Preparation 9

As a resin component, hexamethylene diisocyanate (C, hexamethylene diisocyanate) was mixed with the filler (B) in a weight ratio of 100:1,000 (C:B) to prepare a resin composition.

As the filler (B), a mixture of three types of fillers having different average particle diameters (D50 particle diameter) was applied. Specifically, spherical alumina (B1) having an average particle diameter (D50 particle diameter) of about 70 μm, spherical alumina (B2) having an average particle diameter (D50 particle diameter) of about 20 μm, and average particle diameter (D50 particle diameter) of about 2 μm A filler in which phosphorus non-spherical alumina (B3) was mixed in a weight ratio of 6:1:3 (B1:B2:B3) was used.

<Measurement of abrasion of resin composition>

The abrasion of the resin composition was evaluated using equipment (BUEHLER Beta & Vector) having a shape as shown in FIG. 1 . As shown in FIG. 1 , the equipment has a polishing pad 100 and a rotation pressing means 200 , and a pressing plate 210 is mounted on the rotation pressing means 200 . The surface of the pressure plate 210 has a circular shape as shown in FIG. 2 , and there are five spaces 211 for mounting the wear specimen radially based on the central portion (C). The circular shape of the pressure plate 210 is a circle having a diameter of about 19 to 20 cm, and the distance between the center C of the pressure plate 210 and the space 211 is about 47 mm, and the space ( 211) also has a circular shape with a diameter of about 34 mm. At this time, the distance between the center C of the pressure plate 210 and the space 211 means the distance between the center C of the pressure plate 210 and the center of the space.

In addition, as the pad in the above, Struers MD-Dur whose surface material is woven silk was used. When measuring abrasion, a SUS washer was used as a wear specimen. The SUS washer was made of SUS304 and had a Brinell hardness (KS B 0805) of about 187 HB, and had an inner diameter, an outer diameter, and a thickness of 17 mm, 34 mm and 2 mm, respectively.

100 g of the resin composition was loaded on the pad, and one SUS washer (abrasion specimen) was mounted in one of a plurality of spaces for mounting the wear specimen. The resin composition loaded on the pad was pressed and rotated with a pressure plate equipped with the SUS washer (abrasion specimen). At this time, the pressurization was performed with a pressure of about 10N, and the rotation speed was about 50 rpm. This pressurization was performed for about 10 minutes. In addition, the pressing direction was maintained at an angle of 0 degrees with the normal line of the pad surface, and the rotation axis of the rotation pressing means was performed to maintain an angle of 0 degrees with the direction of the pressing.

Thereafter, the wear amount of the SUS washer was measured by comparing the weight of the polished SUS washer with respect to the initial weight of the SUS washer, and the abrasion degree of the resin composition was evaluated through the wear amount of the SUS washer.

The degree of wear of the resin composition was evaluated as an absolute value of ΔW calculated according to Equation 1 below, and the results of evaluation of the degree of wear of the prepared resin composition are shown in Table 1.

[Formula 1]

△W = (W _f -W _i )/W _i ×100

In Equation 1, W _f is the mass (unit: g) of the wear specimen after pressing is finished, and W _i is the mass (unit: g) of the wear specimen before pressing.

division Wear (%) Preparation Example 1 0.352 Preparation 2 0.370 Preparation 3 0.370 Preparation 4 0.337 Preparation 5 0.929 Preparation 6 0.486 Preparation 7 0.800 Preparation 8 0.396 Preparation 9 0.346

According to the results of Table 1, Preparation Examples 1 to 4, Preparation Examples 8 and 9 showed the absolute value of the wear degree ΔW was 0.45% or less, and Preparation Examples 5 to 7 had the absolute value of the wear degree ΔW. A value greater than 0.45% was shown.

An actual manufacturing process with a static mixer and several injection devices was performed with the resin composition prepared in each Preparation Example. Preparation Examples 1 to 4, Preparation Examples 8 and 9, in which the absolute value of the wear degree ΔW was 0.45% or less, did not damage the static mixer or various injection devices even when the process was performed for a long time, but the absolute value of the wear degree ΔW Preparation Examples 5 to 7, in which the value was 0.45% or less, had a problem in that some equipment was worn as a result of performing the process for a long time.

As such, the method for evaluating abrasion of the resin composition according to the present application can objectively and accurately predict the degree of wear applied by the equipment used in the actual process due to the resin composition when manufacturing the resin composition including the filler. In addition, the method for evaluating the degree of wear of the resin composition may be a method of selecting a resin composition for preventing wear of the equipment or a method of preparing a resin composition for preventing wear of the equipment.

100: pad 210: pressure plate
200: rotation pressing means 220: wear specimen

Claims (13)

Pressing the resin composition present on the pad with a rotary pressing means,
The resin composition includes a resin component and a filler,
The rotational pressing means includes a pressing plate on which a wear specimen is mounted,
The direction of the pressing forms an angle within the range of 0 degrees to 10 degrees with the normal of the pad surface,
The rotational axis of the rotation pressing means is a wear evaluation method forming an angle within the range of 0 degrees to 10 degrees with the direction of the pressing. The method of claim 1, wherein the filler includes inorganic particles having a Mohs hardness of 6 or more. The method of claim 1, wherein the resin composition comprises 80 to 95 wt% of a filler. The method according to claim 1, wherein the filler has a D50 particle diameter in the range of 0.001 to 80 μm. The wear evaluation method according to claim 1, wherein the distance between the rotation shaft of the rotation pressing means and the center of the wear specimen mounted on the pressing plate is in the range of 40 to 60 mm. The method according to claim 1, wherein the wear specimen has a toric shape. [Claim 7] The method of claim 6, wherein the toric-shaped wear specimen has a ratio of an inner diameter to an outer diameter in the range of 1.25 to 5. The method according to claim 1, wherein the wear specimen has a Brinell hardness in the range of 175 to 195 HB. The wear evaluation method according to claim 1, wherein the rotational speed of the rotational pressing means is maintained within a range of 30 to 60 rpm. The wear evaluation method according to claim 1, wherein the pressing is performed at a pressure of 15 N or less. The method of claim 1, wherein the pressing is performed for 3 minutes or more. The wear evaluation method according to claim 1, wherein the wear degree is evaluated according to the following Equation 1:
[Formula 1]
△W = (W _f -W _i )/W _i ×100
In Equation 1, ΔW is the degree of wear (unit: %), W _f is the mass of the wear specimen after pressing (unit: g), and W _i is the mass of the wear specimen before pressing (unit: g). The method according to claim 12, further comprising the step of selecting a resin composition having an absolute value of abrasion ΔW of 0.45% or less.

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