Method for manufacturing a sealing material composition, sealing material composition, and apparatus for manufacturing a sealing material composition

Abstract

This disclosure relates to a method for manufacturing an encapsulant composition, an encapsulant composition, and an apparatus for manufacturing an encapsulant composition. The apparatus and manufacturing method according to this disclosure make it possible to solve the problems of the cumbersome and complex processes inherent in conventional drying techniques, in a situation where the demand for low moisture content in display manufacturing materials is becoming increasingly common and stronger with the development of display technology.

Description

Technical Field

[0001] (Cross - reference to related applications) This application claims the priority and all advantages of U.S. Patent Application No. 63 / 469,881, filed on May 31, 2023, the content of which is incorporated herein by reference in its entirety.

[0002] (Field of the Invention) The present disclosure relates to a method for manufacturing a sealing material composition, a sealing material composition, and a manufacturing apparatus for a sealing material composition.

Background Art

[0003] Sensitivity to moisture is an important issue for electronic devices. Typical electronic devices require humidity levels in the range of less than 1,000 ppm to prevent premature degradation of device performance within a specified operating life or storage life, and some electronic devices require humidity levels in the range of less than 100 ppm.

[0004] Thin film encapsulation (TFE) technology is a technology used to protect organic electroluminescent device (OLED) displays from moisture, oxygen, etc. By applying a thin barrier material on the OLED layer, it is possible to seal the OLED from the environment.

[0005] Generally, as materials for the sealing material composition used in the thin film encapsulation of OLEDs, acrylate - based resins, silicone - based resins, epoxy - based resins, etc. are used, and the sealing material composition is supplied to the thin film encapsulation process. It is common to dry it sufficiently in advance to keep the water content within a certain range.

[0006] If the aqueous phase of the OLED encapsulant composition material is primarily dissolved free water derived from moisture in the air, methods using gravity, merging, and centrifuges for separation are unsuitable. Furthermore, drying techniques for storage, such as headspace dehumidification, forced ventilation, and dry breathers, may also be excluded.

[0007] If the encapsulant composition contains a photoinitiator, it can be easily activated not only by ultraviolet light but also by heat, so heating processes should be avoided. In the case of absorption / adsorption using molecular sieves, pretreatment is almost always required for a high dehydration effect, and there is a problem that the viscosity of the product increases due to chemical contaminants.

[0008] Gas bubbling is the most promising dehydration method, but it is difficult to control. While this technique can easily avoid contamination using inert gases such as nitrogen, it is difficult to establish a stable manufacturing process because the resulting water content after drying is susceptible to atmospheric influences. The design of the drying apparatus must clearly demonstrate water removal performance and allow for control of various variables related to water contamination.

[0009] International Publication No. 2021 / 200668 discloses an OLED sealing composition comprising a (meth)acrylate polymerizable compound and a photopolymerization initiator, with a water content of 1 to 50 ppm. Furthermore, a method for dehydrating the composition by adding a separate desiccant or heating under reduced pressure is disclosed. However, the above-mentioned document does not offer any suggestions for adjusting the water content of an OLED sealing composition containing a silicone resin, which has superior thermal stability, chemical stability, flexibility, and electrical insulation properties compared to acrylate resins.

[0010] Therefore, there is a need for the development of a sealing material composition containing a silicone resin, having a water content of 100 ppm or less, and a dehydration device capable of producing such a sealing material composition. [Prior art documents] [Patent Documents]

[0011] Patent Document 1: International Publication No. 2021 / 200668 [Overview of the project] [Problems that the invention aims to solve]

[0012] The purpose of this disclosure is to provide a sealing material composition having a water content of 100 ppm or less, a manufacturing apparatus for the same, and a method for producing the composition using the apparatus. [Means for solving the problem]

[0013] This disclosure provides a method for producing a sealing material composition having a water content of less than 100 ppm using an apparatus to solve the above problems, wherein the apparatus comprises a drying container having a sparger inserted into a liquid sealing material composition stored in the lower part of the drying container and a sieve tray positioned above the stored liquid sealing material composition; an inert gas supply source for supplying inert gas to the drying container; and a transfer pipe having a first connection part connected to the upper part of the drying container and a second connection part connected to the lower part of the drying container, wherein the method includes supplying inert gas from the inert gas supply source to the liquid sealing material composition through the sparger; aspirating the liquid sealing material composition in the drying container from the second connection part and supplying the aspirated liquid sealing material composition to the first connection part through the transfer pipe; and returning the liquid sealing material composition supplied from the first connection part to the stored sealing material composition through the sieve tray.

[0014] Furthermore, this disclosure provides a sealing material composition comprising a silicone and a silicone organic hybrid oligomer, and a UV curing initiator or a thermosetting catalyst, with a water content of 100 ppm or less.

[0015] Furthermore, this disclosure provides a sealing material composition comprising a silicone and a silicone organic hybrid oligomer and a UV curing initiator or a thermosetting catalyst, wherein the water content is 100 ppm or less and is manufactured by the method described above.

[0016] Furthermore, the present disclosure provides an apparatus for manufacturing a sealing material composition having a water content of 100 ppm or less, comprising: a drying container configured to store a liquid sealing material composition stored in the lower part of the drying container; a sparger inserted into the stored liquid sealing material composition; a sieve tray positioned above the stored liquid sealing material composition; an inert gas supply source configured to supply an inert gas to the stored liquid sealing material composition in the drying container through the sparger; and a transfer pipe having a first connection connected to the upper part of the drying container and a second connection connected to the lower part of the drying container, wherein the transfer pipe is configured to draw the stored liquid sealing material composition through the second connection and supply the drawn liquid sealing material composition through the transfer pipe to the first connection, thereby returning the supplied liquid sealing material composition to the stored sealing material composition through the sieve tray from the first connection. [Effects of the Invention]

[0017] According to this disclosure, in a situation where the demand for low moisture content in display manufacturing materials is becoming increasingly common and stronger with the advancement of display technology, it is possible to solve the problems related to the congestive and complex process concerns inherent in conventional drying technologies. [Brief explanation of the drawing]

[0018] [Figure 1] This figure schematically shows an apparatus according to an embodiment of the present disclosure.

[0019] definition The technical terms used herein are for the purpose of describing specific embodiments and are not intended to limit them. Where used herein, the singular forms “a,” “an,” and “the” are intended to include the plural form unless explicitly indicated in the context. Furthermore, where used herein, the terms “comprises,” “comprising,” “includes,” and / or “including” identify the presence of a described feature, integer, process, operation, element / device, component / constituent, and / or group thereof, but do not exclude the presence or addition of one or more other features, integers, processes, operations, elements / devices, components / constituent, and / or group thereof.

[0020] The use of “for example,” “e.g.,” “such as,” and “including” to list examples is not limited to the examples listed. Therefore, “for example” or “such as” means “for example, but not limited to these” or “such as, but not limited to these,” and includes other similar or equivalent examples. The term “about” as used herein helps to reasonably include or describe slight variations in numerical values ​​measured by instrumental analysis or as a result of handling a sample. Such slight variations may be around ±0 to 25, ±0 to 10, ±0 to 5, or ±0 to 2.5% of the numerical value. Furthermore, the term “about” applies to both numerical values ​​when relating to a range of values. Additionally, the term “about” may apply to numerical values ​​even if not explicitly stated.

[0021] It should be understood that the appended claims are not limited to the obvious and specific compounds, compositions, or methods described in the embodiments for carrying out the invention, and that these may differ between the specific embodiments that fall within the scope of the appended claims. It should be understood that, with respect to any group of Markush on which the description of specific features or aspects of various embodiments relies, different, special, and / or unexpected results may be obtained from each element of each group of Markush independently of all other Markush elements. Each element of a Markush group may be relied upon individually and / or in combination to provide sufficient support for the specific embodiments within the scope of the appended claims.

[0022] When describing various embodiments of the present invention, it should also be understood that any ranges and sub-ranges relied upon are, independently and inclusively, within the scope of the appended claims, and that all ranges, including integer values and / or fractional values, are described and contemplated therein, even if not explicitly written herein. One of ordinary skill in the art will readily recognize that the recited ranges and sub-ranges fully describe and enable various embodiments of the present invention, and that such ranges and sub-ranges can be further delineated into related halves, thirds, quarters, fifths, etc. By way of mere example, the range of "0.1 to 0.9" can be further delineated into the lower third, i.e., 0.1 to 0.3, the middle third, i.e., 0.4 to 0.6, and the upper third, i.e., 0.7 to 0.9, which are, individually and inclusively, within the scope of the appended claims and can individually and / or inclusively rely upon and provide adequate support for particular embodiments within the scope of the appended claims. Additionally, with respect to words that define or modify a range, such as "at least", "more than", "less than", "below", etc., such words are to be understood as including sub-ranges and / or upper or lower limits. As another example, the range of "at least 10" inherently includes sub-ranges of at least 10 to 35, at least 10 to 25, 25 to 35, etc., and each sub-range can individually and / or inclusively rely upon and provide adequate support for particular embodiments within the scope of the appended claims. Finally, individual numbers within the disclosed ranges can rely upon and provide adequate support for particular embodiments within the scope of the appended claims. For example, the range of "1 to 9" includes various individual integers, such as 3, and individual numbers including a decimal point (or fraction), such as 4.1, which can rely upon and provide adequate support for particular embodiments within the scope of the appended claims.

Best Mode for Carrying Out the Invention

[0023] The present disclosure will be described in more detail below. However, this is for merely illustrative purposes and the present disclosure should in no way be construed as limiting the scope of the present disclosure.

[0024] The present disclosure relates to a method for manufacturing a sealing material composition having a water content of less than 100 ppm using a device, the device comprising a drying vessel having a sparger inserted into a liquid sealing material composition stored below the drying vessel and a sieve tray positioned above the stored liquid sealing material composition, an inert gas supply source for supplying an inert gas to the drying vessel, and a transfer pipe having a first connection portion connected to an upper portion of the drying vessel and a second connection portion connected to a lower portion of the drying vessel, the method comprising supplying an inert gas from the inert gas supply source to the liquid sealing material composition through the sparger, sucking the liquid sealing material composition in the drying vessel from the second connection portion, supplying the sucked liquid sealing material composition to the first connection portion through the transfer pipe, and returning the liquid sealing material composition supplied from the first connection portion to the stored sealing material composition through the sieve tray.

[0025] According to the manufacturing method of the present disclosure, a sealing material composition having a water content of 100 ppm or less is provided.

[0026] When a sealing material composition, for example, a composition for OLED sealing, contains an organic solvent such as toluene or is dehydrated using an additive such as a desiccant, the dehydrated composition contains a residual organic solvent or additive. There is a problem that the high purity of the product cannot be guaranteed as a material for manufacturing an OLED. Further, when dehydrating the OLED sealing composition by heating at a high temperature, there is a problem that the photoinitiator contained in the composition is activated by heat.

[0027] Therefore, the present disclosure can provide a sealing material composition that solves various problems while reducing the water content of the sealing material composition to 100 ppm or less using a gas stripping device using gas bubbling.

[0028] The encapsulant composition according to this disclosure may contain silicone and silicone organic hybrid oligomers, and a UV curing initiator or a thermosetting catalyst, but may not contain moisture adsorbents, absorbents, desiccants, or organic solvents.

[0029] Silicon and silicon organic hybrid oligomers are materials that can be used in OLED encapsulant compositions due to their excellent thermal and mechanical properties, high transparency, and low refractive index. Furthermore, they can reduce sensing errors in touch sensors that occur with encapsulants with low electrical conductivity, and low viscosity encapsulants can be applied to OLEDs using inkjet printing technology. This material can be polymerized under a thermosetting catalyst and in the action of a UV curing initiator. According to one embodiment of this disclosure, the silicone and silicon organic hybrid oligomers that can be used include, but are not limited to, polydimethylsiloxane (PDMS), polyphenylsilsesquioxane (PPSQ), methylphenylsilicone (MPS), polyhedral oligomeric silsesquioxane (POSS), and vinyl-terminated silicone resin (VTSR).

[0030] The UV curing initiator is not particularly limited as long as it can induce polymerization of the silicones and silicone organic hybrid oligomers described above. According to one embodiment of this disclosure, the UV curing initiator may be, for example, a cationic photopolymerization initiator, a photoradical polymerization initiator, and the like.

[0031] Examples of thermosetting catalysts include imidazole derivatives, such as imidazole, 2-methylimidazole, 2-ethylimidazole, 2-ethyl-4-methylimidazole, 2-phenylimidazole, 4-phenylimidazole, 1-cyanoethyl-2-phenylimidazole, and 1-(2-cyanoethyl)-2-ethyl-4-methylimidazole; amines, such as dicyandiamide, benzyldimethylamine, 4-(dimethylamino)-N,N-dimethylbenzylamine, 4-methoxy-N,N-dimethylbenzylamine, and 4-methyl-N,N-dimethylbenzylamine; hydrazine compounds, such as adipic acid dihydrazide and sebacate acid dihydrazide; and phosphorus compounds, such as triphenylphosphine. Furthermore, guanamine, acetoguanamine, benzoguanamine, melamine, and other S-triazine derivatives, such as 2,4-diamino-6-methacryloyloxyethyl-S-triazine, 2-vinyl-2,4-diamino-S-triazine, 2-vinyl-4,6-diamino-S-triazine isocyanuric acid adduct, and 2,4-diamino-6-methacryloyloxyethyl-S-triazine isocyanuric acid adduct, may be used, but are not limited to these.

[0032] The sealing material compositions of this disclosure do not necessarily contain moisture adsorbents, absorbents, desiccants, and organic solvents. Moisture adsorbents, absorbents, desiccants, and organic solvents can refer to additives commonly used in the art to reduce the water content of the sealing material composition. Examples of moisture adsorbents include calcium oxide (CaO), barium oxide (BaO), zeolites, silica gel, molecular sieves, montmorillonite, sodium hydroxide (NaOH), and potassium hydroxide (KOH). Examples of organic solvents include glycol-based organic solvents.

[0033] Conventional encapsulant compositions generally contain additives such as water adsorbents, absorbents, desiccants, and organic solvents to effectively reduce the water content in the dehydration process, and these additives have been adequately removed by a filtration process after dehydration. However, since it is impossible to completely remove additives already present in the encapsulant composition, the encapsulant composition before being supplied to the thin-film encapsulation process contains small amounts of residual additives or requires filtration and filtration processes. When encapsulating OLEDs with such low-purity encapsulant compositions, impurities may escape during the manufacturing process, potentially resulting in dead cells, which in turn can prevent the OLED pixels from functioning, thus limiting the protection of the OLED from moisture and oxygen. Therefore, this disclosure has the advantage of being able to provide encapsulant compositions with a water content of 100 ppm or less without using additives such as water adsorbents, absorbents, desiccants, and organic solvents.

[0034] The sealing material composition according to this disclosure may further comprise an epoxy compound. Examples of epoxy compounds include, but are not limited to, 3-glycidoxypropyltrimethoxysilane, 3-glycidoxypropylmethyldimethoxysilane, 3-glycidoxypropyltriethoxysilane, 3-glycidoxypropylmethyldiethoxysilane, 2-(3,4-epoxycyclohexyl)ethyltrimethoxysilane, 2-(3,4-epoxycyclohexyl)ethylmethyldimethoxysilane, and 2-(3,4-epoxycyclohexyl)ethyltriethoxysilane.

[0035] According to one embodiment of the present disclosure, the encapsulant composition of the present disclosure may further contain, in appropriate amounts, other components such as surfactants, photosensitizers, antioxidants, and ultraviolet stabilizers, without impairing the purpose of the present disclosure.

[0036] The encapsulant composition of this disclosure may be used for encapsulating OLEDs. The cured product of this disclosure can be obtained by irradiating the aforementioned encapsulant composition with ultraviolet light, and the OLED of this disclosure can be sealed with the cured material. The encapsulant composition can be applied to an OLED by methods known in the art, such as vapor deposition, coating, or inkjet printing, and can be cured by ultraviolet irradiation to form a cured product that encapsulates the OLED.

[0037] The apparatus used in the manufacturing method of this disclosure will be described below.

[0038] The apparatus of this disclosure may be operated in a closed system. The drying apparatus is a closed system that prevents the intrusion of air from the atmosphere and controls the release of asphyxiating gases into designated vent lines. The drying unit is designed to perform both filtration and drying. In some cases, drying and filtration may need to be performed separately. In this specification, the dried product must be stored without re-contamination of moisture during filtration or before packaging. A closed system is capable of essentially maintaining the quality of the moisture content.

[0039] Hereinafter, embodiments of the apparatus described herein will be explained with reference to the drawings.

[0040] In this disclosure, the singular form includes the plural form unless otherwise specified herein. For example, as used herein, "sieve tray" may mean at least one of the first sieve tray and the second sieve tray, and "sparger" may mean at least one of the first sparger and the second sparger.

[0041] Figure 1 is a schematic diagram showing an apparatus according to an embodiment of the present disclosure.

[0042] Referring to Figure 1, an apparatus according to one embodiment of the present disclosure comprises a drying container, an inlet for the sealing material composition, an inert gas supply source, a vent, a sparger, a sieve tray, a transfer pipe, and the like.

[0043] The drying vessel is provided to serve as a reaction vessel in which the dehydration process of the encapsulant composition takes place, and may be configured as a closed system to block the penetration of moisture from the air. The inflow and outflow of the encapsulant composition, moisture trapped within the encapsulant composition, and inert gas can be controlled by an inlet for the encapsulant composition, an inert gas supply source, a sparger, and a vent connected to the drying vessel.

[0044] The drying vessel may also be a pressurized vessel. The drying performance is proportional to the flow rate of the drying gas, and the convergence value is determined by the flow rate. Therefore, since the flow rate needs to be adjusted as needed, the drying vessel may be a pressurized vessel for inherent safety reasons. Assuming that the main supply pressure of the inert gas is 7 bar, the design pressure can be higher than 10 bar. The drying gas is the inert gas of this disclosure and may be nitrogen or the like.

[0045] The size of the drying container can be determined considering the volume of the product, the space in the sieve tray, and the fact that if bubbles are continuously bubbled, a large amount of air bubbles will be generated and can move to the upper vent line, thus requiring extra space. However, if the extra space is too large, it may impair the performance of the sieve tray.

[0046] The inlet for the sealing material composition is provided for supplying the sealing material composition to the drying container and may be located in the upper part of the drying container.

[0047] The inert gas of this disclosure is supplied from an inert gas source and injected into a drying vessel through a sparger, and a vent is located at the top of the drying vessel to discharge the inert gas from the drying vessel. The vent line is designed to conveniently control the gas flow with a valve. In the initial design stage, the size of the vent line can be set to allow the flow of inert gas at, for example, 50 to 200 NL / min.

[0048] The drying container comprises a sparger inserted into the liquid sealant composition stored at the bottom, and a sieve tray positioned on the stored liquid sealant composition.

[0049] A sparger is a nozzle for supplying an inert gas to a drying container. In this specification, the smaller the bubble size, the larger the contact area between the liquid and gas for mass transfer. Therefore, the sparger may be a sintered metal filter having a pore diameter of 100 μm or less. According to one embodiment of this disclosure, the pore diameter may be 0.2 to 100 μm. When an inert gas is injected into a sealing material composition through a sintered metal filter having one or more pores, the dewatering effect of the sealing material composition is further improved by increasing the contact area between the sealing material composition and the inert gas. The number and length of the spargers are adjusted to minimize wasted volume in the container. The volume per unit size of the sparger may affect the drying performance. The shape of the sparger may also vary and may have a circular shape, a bottom shape, etc., but is not limited to these.

[0050] The sieve tray has one or more openings to increase the contact area between the sealing material composition and the inert gas, thereby improving the efficiency of mass transfer between the liquid and the gas. Moisture in the sealing material composition of this disclosure changes from liquid to gas, and the gas containing the moisture then moves upward. Meanwhile, the gas passes through the air layer at the liquid surface and exits to the vent line. In this specification, the recirculated liquid falls from the top to the bottom of the drying container, and the gas rises through the same openings of the sieve tray, coming into contact with each other while backflowing in the sieve tray. Mass transfer occurs through the contact between the liquid and the gas. This mass transfer is effective in transporting the gas containing moisture to the vent line. To maximize mass transfer efficiency, it is recommended to use all openings of the sieve tray. The size of the openings of the sieve tray may vary depending on the flow rate and viscosity of the liquid to be stored.

[0051] In this specification, a return line may be further provided between the sieve tray and the first connection portion to uniformly distribute the supplied sealing material composition onto the sieve tray.

[0052] Furthermore, the drying container is equipped with a transfer pipe having a first connection part connected to the upper part of the drying container and a second connection part connected to the lower part of the drying container.

[0053] The transfer pipe is configured to draw the stored liquid sealant composition through a second connection and supply the drawn liquid sealant composition through the transfer pipe to a first connection, thereby returning the supplied liquid sealant composition from the first connection through the sieve tray to the stored sealant composition.

[0054] The transfer pipe may further include a pump for circulating the liquid sealant composition. The pump raises the sealant composition supplied to the lower part of the drying container and circulates it to the upper part of the drying container, and may be located outside the drying container.

[0055] Furthermore, the apparatus of this disclosure may include a stirrer, a level switch, a vacuum pump, a recirculation pump, a filter, and the like.

[0056] In the manufacturing method of the present disclosure, once foam is formed and grows, the foam moves rapidly through the vent line. Since the foam contains a large amount of liquid, it can cause process problems, including significant losses and safety issues. Therefore, a stirrer and a level switch can be used to break the foam, prevent foam growth, or prevent liquid from falling from above due to recirculation from the growing foam. The height of the stirrer may be the height of the top surface of the liquid encapsulant composition of the present disclosure to facilitate foam breakdown.

[0057] Vacuum not only accelerates mass transfer but also breaks bubbles, so vacuum pumps can be used.

[0058] A recirculation pump can perform several functions. Firstly, it circulates the liquid from the bottom to the top of the drying container for mass transfer within the sieve tray. Secondly, it circulates the liquid for filtration. The liquid needs to be recirculated for several hours to filter out dust from the total volume of liquid. Thirdly, the pump helps fill the drying container with liquid from the drum. Finally, the pump helps feed the purified and dried product to the packaging machine.

[0059] The manufacturing method of the present disclosure includes supplying an inert gas from an inert gas supply source to a liquid sealant composition through a sparger; drawing the liquid sealant composition in a drying container from a second connection and supplying the drawn liquid sealant composition to a first connection through a transfer pipe; and returning the liquid sealant composition supplied from the first connection to the stored liquid sealant composition through a sieve tray.

[0060] The detailed explanation of each process corresponds to the description of the equipment.

[0061] The manufacturing method disclosed herein does not necessarily have to include a heating process.

[0062] Conventionally, it has been common practice to heat and dry encapsulant compositions. However, when encapsulant compositions are heated to a temperature of 40°C or higher, the photopolymerization initiator contained in the encapsulant composition is activated by the heat, thereby increasing the viscosity of the encapsulant composition. Therefore, the manufacturing method of the present disclosure does not include a heating process, thereby preventing the activation of the photopolymerization initiator during the drying process of the encapsulant composition.

[0063] This disclosure demonstrates that by controlling the water content of the encapsulant composition to 100 ppm or less before supplying it to a known thin-film process, chemical damage to the OLED can be prevented even when the cured encapsulant composition is directly deposited or coated onto the OLED to seal it, thereby improving the reliability of the OLED.

[0064] On the other hand, silicone resins are superior to acrylate resins in terms of thermal stability, chemical stability, flexibility, and electrical insulation. When encapsulating an OLED using an encapsulating material composition containing silicone resin, it is possible to manufacture an OLED with superior durability and the ability to operate without malfunction using a smaller amount of coating. Therefore, by reducing the water content of the encapsulating material composition containing silicone resin to 100 ppm or less, the OLED encapsulated using the encapsulating material composition of this disclosure can exhibit superior effects in terms of light output, mechanical properties, and reliability.

[0065] The following describes a method for producing a sealing material composition with a water content of 100 ppm or less using the apparatus, and specific embodiments of the apparatus according to this disclosure. However, the following examples are merely illustrative of this disclosure for a detailed understanding of it, and this disclosure is not limited to the following examples. [Examples]

[0066] The UV-curable organopolysiloxane composition for OLEDs was dried. Specifically, the apparatus and operating conditions used in the examples are as follows.

[0067] The apparatus for dewatering the encapsulant composition comprises a drying container, an inlet for the encapsulant composition, a vent, a pump, a sparger, and a sieve tray. The structure and operation of the dewatering apparatus, as well as the method for manufacturing the dewatered encapsulant composition, are the same as described above, so redundant explanations will be omitted. Below, we will describe the specific structure of the device and the results of the water content of the encapsulant composition dewatered by the apparatus.

[0068] The sealing material composition, before dewatering, was injected in 10 kg quantities from the drum into the upper line of the drying vessel via piping connected to a pump, and then transferred to a 20 L drying vessel. The sealing material composition transferred to the drying vessel was continuously circulated, being moved back to the top of the drying vessel via the pump. Nitrogen was injected through a sparger located at the bottom of the drying vessel.

[0069] To facilitate mixing with nitrogen through a smooth flow of the sealant composition within the drying vessel, the second connection point within the drying vessel is positioned on the lower side. The injected sealant composition was poured into the center of the sieve tray to ensure good dispersion. The apparatus used was equipped with a single sparger of a φ25.4 mm × 214 mm sintered filter with pores of 1 micron in size. Nitrogen as a dry gas was injected at a flow rate of 90 NL / min for approximately 5 hours.

[0070] Three sieve trays, each having 86 openings with a diameter of 12.7 mm and a constant distance between each opening, were placed on top of the drying container. The distance between the sieve trays was 38 mm, and the distance between the top of the drying container and the sieve trays was also 38 mm. In two adjacent sieve trays, each sieve tray was configured to increase contact between the sealant composition and nitrogen gas by ensuring that the openings were not collinear with respect to the vertical. The moisture-containing gas comes into contact again with the recirculating sealant composition falling through the sieve tray by mass transfer as it passes through the sealant. Through this process, the moisture-containing nitrogen gas flows out of the drying container through a vent line.

[0071] Using the apparatus and manufacturing method described above, an ultraviolet-curable organopolysiloxane composition having the composition (parts by mass) shown in Table 1 below was dried.

[0072] Component (A) is (EpMe2Si)2O (wherein "Ep" is epoxy and "Me" is methyl).

[0073] Component (B) is EpMeSi(OSiMe3)2.

[0074] Component (C) is a combination of 96 parts of component (X) and 4 parts of component (Y) (component (X) is 4-isopropyl-4'-methyldiphenyliodonium tetrakis(pentafluorophenyl)borate, and component (Y) is 2-isopropylthioxanthone).

[0075] [Table 1]

[0076] After drying, the UV-curable organopolysiloxane compositions of Examples 1-3 had water contents of 64.8 ppm, 62.7 ppm, and 57.9 ppm, respectively.

Claims

1. A method for producing a sealing material composition with a water content of less than 100 ppm using an apparatus, wherein the apparatus comprises: a drying container having a sparger inserted into a liquid sealing material composition stored in the lower part of the drying container and a sieve tray positioned above the stored liquid sealing material composition; an inert gas supply source for supplying inert gas to the drying container; and a transfer pipe having a first connection part connected to the upper part of the drying container and a second connection part connected to the lower part of the drying container, wherein the method is The inert gas from the inert gas supply source is supplied to the liquid sealing material composition through the sparger, The liquid sealing material composition in the drying container is drawn out from the second connection, and the drawn liquid sealing material composition is supplied to the first connection through the transfer pipe. A method comprising returning the liquid sealing material composition supplied from the first connection to the stored sealing material composition through the sieve tray.

2. The method according to claim 1, wherein the sealing material composition comprises silicone and a silicone organic hybrid oligomer and a UV curing initiator or a thermosetting catalyst, and does not contain a moisture adsorbent, absorbent, desiccant, or organic solvent.

3. The method according to claim 1, wherein the sparger is a sintered metal filter having pores, and the size of the pores of the sintered metal filter is 100 μm or less.

4. The method according to claim 1, wherein the method does not include a heating process.

5. The method according to claim 1, wherein the drying container further comprises a vent, the vent being positioned above the drying container to discharge the inert gas from the drying container.

6. A sealing material composition comprising silicone and silicone organic hybrid oligomer, and a UV curing initiator or thermosetting catalyst, wherein the water content is 100 ppm or less.

7. A sealing material composition comprising a silicone and a silicone organic hybrid oligomer and a UV curing initiator or a thermosetting catalyst, wherein the water content is 100 ppm or less, and the sealing material composition is manufactured by the method described in claim 1.

8. The sealing material composition according to claim 7, wherein the sealing material composition does not contain a moisture adsorbent, an absorbent, a desiccant, and an organic solvent.

9. The sealing material composition according to claim 7, wherein the sealing material composition further comprises an epoxy compound.

10. The sealing material composition according to claim 7, wherein the sealing material composition is for sealing an organic electroluminescent element.

11. A manufacturing apparatus for a sealing material composition having a water content of 100 ppm or less, A drying container configured to store a liquid sealing material composition stored in the lower part of the drying container, A spar inserted into the stored liquid sealing material composition, A sieve tray positioned above the stored liquid sealing material composition, An inert gas supply source configured to supply the inert gas to the stored liquid sealing material composition in the drying container through the sparger, An apparatus comprising a transfer pipe having a first connection part connected to the upper part of the drying container and a second connection part connected to the lower part of the drying container, wherein the transfer pipe is configured to suck the stored liquid sealing material composition through the second connection part and to supply the sucked liquid sealing material composition through the transfer pipe to the first connection part, thereby returning the supplied liquid sealing material composition from the first connection part through the sieve tray to the stored sealing material composition.

12. The apparatus according to claim 11, wherein the sparger is a sintered metal filter having pores, and the size of the pores of the sintered metal filter is 100 μm or less.

13. The apparatus according to claim 11, wherein the transfer pipe further comprises a pump for circulating the liquid sealing material composition.

14. The apparatus according to claim 11, further comprising a return line disposed between the first connection and the sieve tray for uniformly distributing the supplied sealing material composition across the sieve tray.

15. The apparatus according to claim 11, wherein the drying container further comprises a vent, the vent being positioned above the drying container to discharge the inert gas from the drying container.

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