Method and device for mechanical separation of multiple interlayers - Patents.com

Abstract

A process is disclosed for separating a first layer of a multi-layer interlayer sheet from a remainder, in which the multi-layer sheet is heated and then the first layer of the multi-layer interlayer sheet is separated from the remainder by pulling the first layer and the remainder in different directions in a defined orientation.

Description

[Background technology]

[0001]

[0001] Multi-layer interlayers continue to gain a larger share of the interlayer market, but their recyclability in the extrusion process is limited because different layers may have different physicochemical properties. The acoustic core layer in particular does not mix well with the two skin layer materials during extrusion, forming small but discrete domains of the core material, which causes a certain level of haze, thus limiting its content in the extrusion. The inability to reprocess this multi-layer material represents a significant economic loss.

[0002]

[0002] To demonstrate the concept of mechanical separation, it is possible to manually peel the skin layers from multi-layer sheets, but improved processes and mechanical devices would be useful for stable, consistent, and cost-effective mechanical separation operations.

[0003]

[0003] US Patent 5,368,978 discloses a method of stripping an imaging material comprising the steps of providing an imaging material including a donor element and a receiver element, heating the imaging material, applying opposing forces to the donor element and the receiver element to separate the imaging material into a donor element and a receiver element, and accumulating the separated donor element. In a preferred method, one or both of the opposing forces is a vacuum, and when the vacuum is released from the donor element, accumulation occurs by winding after separation. An apparatus for stripping an imaging material includes a means for applying heat and pressure to the imaging material, a means for applying a separation force to at least one of the donor element and the receiver element forming the imaging material, and a means for separating the donor element and the receiver element. In a preferred embodiment, the apparatus further includes a means for winding the donor element and a means for preheating the imaging material before applying the separation force.

[0004]

[0004] US Patent No. 5,934,577 discloses a process for separating components of a multi-layer material comprising at least one layer of base plastic (A) and a layer of plastic (B) separated by a layer of sticky plastic (C), in which (1) the material is heated to a temperature T1 between the crystallization temperature (Tc) of plastic B and Tc-20°C, (2) the material is then subjected to shear at about the same temperature to shred, thereby causing delamination and converting the material into two types of small sized particles, some of which (X) consist essentially of base plastic (A) and others (Y) consist essentially of plastic B and sticky plastic (C), and (3) particles X and Y are then separated by electrostatic separation.

[0005]

[0005] U.S. Patent No. 10,513,102 discloses a peeling device including a transport roller configured to transport a laminate in which a first substrate having an opening and a second substrate are peelably laminated, a peeling roller arranged opposite the transport roller across the laminate and configured to peel the second substrate from the first substrate, a take-up roller arranged spaced apart from the peeling roller and configured to take up the second substrate peeled from the first substrate, and a wind-up auxiliary roller arranged between the peeling roller and the take-up roller and having a stepped portion for maintaining the width of the opening.

[0006]

[0006] U.S. Patent Application Publication No. 2020 / 0147933 discloses a method for recycling an intermediate film for laminated glass, the method including a step of separating a layer including layer A and a layer including layer B from an intermediate film for laminated glass (1) including at least layer A and layer B. Summary of the Invention [Problem to be solved by the invention]

[0007]

[0007] There remains a need for methods and devices for separating layers of multi-layer interlayers to facilitate reworking of the material in the manufacturing process. Similarly, there remains a need for obtaining polymer sheets, particularly PVB sheets, having smoother surfaces than those obtainable using conventional extrusion techniques. [Means for solving the problem]

[0008]

[0008] The present invention relates to a continuous process for separating a first layer of a multilayer interlayer sheet from a remainder, the process comprising the steps of heating the multilayer sheet to an elevated temperature and thereafter separating the first layer of the multilayer interlayer sheet from a remainder by pulling the first layer and the remainder of the multilayer interlayer sheet in different directions. According to this aspect, during the continuous process, an angle α defined by the first layer and the multilayer sheet at a point of separation is less than or equal to an angle β defined by the multilayer sheet at the point of separation and the remainder of the multilayer sheet.

[0009]

[0009] The present invention also relates to a continuous process for separating a first layer of a multilayer interlayer sheet from a remaining portion thereof, the process comprising the steps of heating the multilayer sheet to an elevated temperature and thereafter separating the first layer of the multilayer interlayer sheet from a remaining portion thereof by pulling the first layer and the remaining portion of the multilayer interlayer sheet in different directions in an orientation. According to the present invention, an angle α is defined by the first layer and the multilayer sheet at the separation point, an angle β is defined by the multilayer sheet at the separation point and the remaining portion of the multilayer sheet, and an angle γ is defined by the first layer and the remaining portion of the multilayer sheet at the separation point, such that the following formula is satisfied: β / α≧1 30°≦γ≦180° α+β+γ=360°

[0010] According to the present invention, the above orientation is maintained during the continuous process.

[0010]

[0011] In another aspect, the present invention relates to an apparatus for carrying out the method of the present invention.

[0011]

[0012] Further aspects of the invention are as disclosed and claimed herein. [Brief description of the drawings]

[0012] [Figure 1] FIG. 1 is a schematic diagram of a method for mechanically recycling a multi-layer interlayer. [Diagram 2] FIG. 2 is a schematic diagram of a device according to the invention for mechanically separating a multi-layer interlayer. [Diagram 3] FIG. 1 is a schematic diagram showing the proper orientation of the film while being separated. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0013] The following embodiments and combinations are included within the scope of the present invention: 1. A continuous process for separating a first layer from a remainder of a multi-layer interlayer sheet, comprising: a. heating the multilayer sheet to a temperature of about 25° C. to about 70° C.; and b. thereafter, separating the first layer of the multilayer interlayer sheet from the remainder by pulling the first layer and the remainder of the multilayer interlayer sheet in different directions, wherein during the continuous process, an angle α defined by the first layer and the multilayer sheet at the separation point is less than or equal to an angle β defined by the multilayer sheet at the separation point and the remainder of the multilayer sheet. 2. The continuous process of embodiment 1, wherein during the continuous process, angle α is smaller than angle β. 3. The process of any of the preceding embodiments, wherein angle α is at least 30 degrees less than angle β. 4. The process of any of the previous embodiments, wherein angle α is at least 50 degrees less than angle β. 5. The process of any of the previous embodiments, wherein angle α is at least 60 degrees less than angle β. 6. The process of any of the previous embodiments, wherein angle α is at least 75 degrees less than angle β. 7. The process of any of the preceding embodiments, wherein angle α is about 10 degrees to about 100 degrees less than angle β. 8. The process of any of the preceding embodiments, wherein angle α is about 30 degrees to about 75 degrees less than angle β. 9. The process of any of the previous embodiments, wherein the first layer comprises a poly(vinyl butyral) polymer having a Tg of about 25° C. to about 40° C. 10. The process of any of the preceding embodiments, wherein the multilayer sheet is heated in step a) to a temperature of from 30° C. to 70° C. 11. The process of any of the previous embodiments, wherein at least a portion of the remainder of the multilayer sheet comprises a poly(vinyl butyral) polymer having a Tg at least 15° C. lower than the Tg of the first layer. 12. In a separating step, the first layer is pulled by a first layer pull roll, and the remaining portion of the multi-layer interlayer sheet is pulled by a remaining portion pull roll; The process of any of the preceding embodiments, wherein the distance between the first layer pull roll and the remainder portion pull roll is maintained at less than about 50% of the width of the sheet while separation is occurring. 13. The process of any of the preceding embodiments, further comprising cooling the one or more first layers and the remainder of the multilayer sheet below the Tg of the poly(vinyl butyral) of the first layer or the Tg of the poly(vinyl butyral) of the remainder of the multilayer sheet. 14. The process of any of the preceding embodiments, further comprising cooling the first layer to a temperature of about 15°C to about 30°C. 15. The process of any of the preceding embodiments, further comprising cooling the remaining portion of the multilayer sheet to a temperature of about -15°C to about 0°C. 16. The process of any of the preceding embodiments, wherein the distance between the first layer pull roll and the remainder portion pull roll during separation is less than about 15% of the width of the sheet. 17. The process of any of the preceding embodiments, wherein the distance between the first layer pull roll and the remainder portion pull roll during separation is less than about 5% of the width of the sheet. 18. The process of any of the preceding embodiments, wherein the multilayer sheet includes a core layer having skin layers on each side. 19. The process of any of the previous embodiments, wherein the first layer comprises a first skin layer, the first skin layer being thicker than the other skin layer. 20. The process of any of the previous embodiments, wherein the first layer comprises a first skin layer, the first skin layer being thinner than the other skin layer. 21. The process of any of the preceding embodiments, wherein the first end of the multi-layer sheet is thicker than the second end of the multi-layer sheet. 22. A continuous process for separating a first layer from a remainder of a multi-layer interlayer sheet, comprising: a. heating the multilayer sheet to a temperature of about 25° C. to about 70° C.; and b. thereafter, separating the first layer of the multilayer interlayer sheet from the remainder by pulling the first layer and the remainder of the multilayer interlayer sheet in different directions in an orientation, wherein an angle α is defined by the first layer and the multilayer sheet at the separation point, an angle β is defined by the multilayer sheet and the remainder of the multilayer sheet at the separation point, and an angle γ is defined by the first layer and the remainder of the multilayer sheet at the separation point, and the angle α is determined by the first layer and the remainder of the multilayer sheet according to the following formula: β / α≧1 30°≦γ≦180° α+β+γ=360° Fulfilling A process in which the orientation is maintained during a continuous process. 23. The continuous process of any of the preceding embodiments, wherein during the continuous process, angle α is smaller than angle β. 24. The process of any of the previous embodiments, wherein angle α is at least 30 degrees less than angle β. 25. The process of any of the previous embodiments, wherein angle α is at least 50 degrees less than angle β. 26. The process of any of the previous embodiments, wherein angle α is at least 60 degrees less than angle β. 27. The process of any of the previous embodiments, wherein angle α is at least 75 degrees less than angle β. 28. The process of any of the previous embodiments, wherein angle α is about 10 degrees to about 100 degrees less than angle β. 29. The process of any of the preceding embodiments, wherein angle α is between about 30 degrees and about 75 degrees less than angle β. 30. The process of any of the previous embodiments, wherein the first layer comprises a poly(vinyl butyral) polymer having a Tg of about 25°C to about 40°C. 31. The process of any of the preceding embodiments, wherein the multilayer sheet is heated in step a) to a temperature of from 30° C. to 70° C. 32. The process of any of the previous embodiments, wherein at least a portion of the remainder of the multilayer sheet comprises a poly(vinyl butyral) polymer having a Tg at least 15° C. lower than the Tg of the first layer. 33. In a separating step, the first layer is pulled by a first layer pull roll, and the remaining portion of the multi-layer interlayer sheet is pulled by a remaining portion pull roll; The process of any of the preceding embodiments, wherein the distance between the first layer pull roll and the remainder portion pull roll is maintained at less than about 50% of the width of the sheet while separation is occurring. 34. The process of any of the preceding embodiments, further comprising cooling the one or more first layers and the remainder of the multilayer sheet below the Tg of the poly(vinyl butyral) of the first layer or the Tg of the poly(vinyl butyral) of the remainder of the multilayer sheet. 35. The process of any of the previous embodiments, further comprising cooling the first layer to a temperature of about 30°C to about 15°C. 36. The process of any of the previous embodiments, further comprising cooling the remaining portion of the multilayer sheet to a temperature of about -15°C to about 0°C. 37. The process of any of the preceding embodiments, wherein the distance between the first layer pull roll and the remainder portion pull roll during separation is less than about 15% of the width of the sheet. 38. The process of any of the preceding embodiments, wherein the distance between the first layer pull roll and the remainder portion pull roll during separation is less than about 5% of the width of the sheet. 39. The process of any of the preceding embodiments, wherein the multilayer sheet includes a core layer having skin layers on each side. 40. The process of any of the previous embodiments, wherein the first layer comprises a first skin layer, the first skin layer being thicker than the other skin layer. 41. The process of any of the previous embodiments, wherein the first layer comprises a first skin layer, the first skin layer being thinner than the other skin layer. 42. The process of any of the preceding embodiments, wherein the first end of the multi-layer sheet is thicker than the second end of the multi-layer sheet.

[0014]

[0014] The following embodiments and combinations are also within the scope of the present invention. 1. Embodiment 1. A poly(vinyl acetal) film comprising a smooth side exhibiting an Rz of about 0 to about 10, and a rough side opposite the smooth side exhibiting an Rz of about 10 to about 150. 2. The poly(vinyl acetal) film of embodiment 1, wherein the rough surface exhibits an Rz of about 10 to about 100 and results from melt fracture. 3. The poly(vinyl acetal) film of any of the preceding embodiments, wherein the rough surface exhibits an Rz of about 10 to about 150 and results from melt fracture and embossing. 4. The poly(vinyl acetal) film of any of the previous embodiments, wherein the film comprises poly(vinyl butyral). 5. The poly(vinyl acetal) film of any of the preceding embodiments, wherein the poly(vinyl butyral) is plasticized and has a Tg of about 20°C to about 40°C. 6. The poly(vinyl acetal) film of any of the previous embodiments, wherein the poly(vinyl butyral) has a hydroxyl content of about 10% to about 30% by weight. 7. a. forming at least a first polymer melt and a second polymer melt; b. co-extruding at least a first polymer melt and a second polymer melt to form a multi-layer intermediate layer including a first layer and a remainder of the multi-layer sheet including a second layer, the multi-layer sheet having a surface roughness imparted by melt fracture on an outer surface thereof during co-extrusion; and c. thereafter, separating the first layer from the remainder of the multi-layer interlayer sheet by pulling the first layer and the remainder of the multi-layer interlayer sheet in different directions. 3. The poly(vinyl acetal) film of any of the preceding embodiments, produced by a process comprising: 8. The poly(vinyl acetal) film of any of the previous embodiments, wherein the first polymer melt and the second polymer melt comprise poly(vinyl butyral). 9. a. forming a first polymer melt comprising at least poly(vinyl butyral) and a second polymer melt comprising a sulfopolyester; and b. co-extruding at least a first polymer melt and a second polymer melt to form a multi-layer intermediate layer including the first layer and a remainder of the multi-layer sheet including the second layer, the multi-layer sheet having a surface roughness imparted by melt fracture on an outer surface thereof during co-extrusion; and c. thereafter, separating the first layer from the remainder of the multi-layer interlayer sheet by dissolving the sulfopolyester. 3. The poly(vinyl acetal) film of any of the preceding embodiments, produced by a process comprising: 10. The poly(vinyl acetal) film of any of the previous embodiments, wherein the second polymer melt comprises a sulfopolyester. 11. a. forming at least a first polymer melt and a second polymer melt; b. co-extruding at least the first polymer melt and the second polymer melt to form a multi-layer intermediate layer including the first layer and a remainder of the multi-layer sheet including the second layer; c. embossing the multilayer sheet to obtain a multilayer sheet having a surface roughness on its outer surface; and d. thereafter, separating the first layer from the remainder of the multi-layer interlayer sheet by pulling the first layer and the remainder of the multi-layer interlayer sheet in different directions. 3. The poly(vinyl acetal) film of any of the preceding embodiments, produced by a process comprising: 12. The poly(vinyl acetal) film of any of the preceding embodiments, wherein the coextrusion comprises coextruding through a multi-manifold die having at least two die manifolds, and at least a first polymer melt and a second polymer melt are extruded through separate die manifolds. 13. The poly(vinyl acetal) film of any of the preceding embodiments, wherein in the separation step, the angle α defined by the first layer and the multilayer sheet at the separation point is less than or equal to the angle β defined by the multilayer sheet at the separation point and the remainder of the multilayer sheet during the continuous process. 14. The poly(vinyl acetal) film of any of the previous embodiments, wherein angle α is less than angle β during continuous processing. 15. The poly(vinyl acetal) film of any of the previous embodiments, wherein angle α is at least 30 degrees less than angle β. 16. The poly(vinyl acetal) film of any of the preceding embodiments, wherein angle α is about 30 degrees to about 75 degrees less than angle β. 17. The process of any of the preceding embodiments, wherein the multilayer sheet is heated in step a) to a temperature of from 30° C. to 70° C. 18. The process of any of the preceding embodiments, wherein the distance between the first layer pull roll and the remainder portion pull roll during separation is less than about 15% of the width of the sheet.

[0015]

[0015] The separation process according to the present invention may be described herein as continuous, but the term "continuous" is not intended to be limiting. Those skilled in the art of industrial processes will understand that a continuous process is distinct from a batch process, and that the longer the process can be maintained continuously, the greater the advantage in terms of throughput. Thus, the advantage of the process of the present invention is that, at steady state, the multi-layered sheet roll can be continuously separated for a significant period of time, and the present disclosure allows those skilled in the art to adjust the process to maintain the desired continuity when running the process. Thus, the present invention and claims are intended to encompass any process that may be artificially interrupted or disturbed to prevent the process from being run continuously.

[0016]

[0016] Other embodiments are as disclosed and claimed herein.

[0017]

[0017] Thus, the present invention relates to a method and device for separating two layers of a multi-layer intermediate layer by (i) unwinding the intermediate layer from the roller, (ii) heating the intermediate layer with one or more heated rollers and / or a separate IR heater, (iii) peeling the first layer or skin layer under a separating force, and (iii) collecting the separated skin layer and the remaining portion of the multi-layer sheet, which are then reused as an intermediate layer component.

[0018] In another aspect, the present invention relates to a method and device design for separating the core and skin materials of a multi-layered interlayer, e.g. with a roll width of 1.4 m and roll weight up to 500 kg, by mechanically peeling one skin layer at a speed of e.g. 2-20 m / min, so that the recovered skin layers can be reused in extrusion. See Figure 1, which shows a core layer and an interlayer with two skin layers.

[0019] The present invention thus relates to a method and device capable of mechanically separating a first or skin layer from a multilayer interlayer sheet (e.g., Eastman's Saflex™ PVB interlayer). Thus, while the goal is to mechanically separate one skin layer from the core-skin bilayer of a three-layer acoustical interlayer, the scope of processable materials of the device disclosed herein is not limited to three layers, but includes multilayer interlayers in which the number of layers is greater than two, or greater than three, or greater than five, or greater than five layers, either partially or fully across the width of the sheet. In either case, separation typically occurs between the skin layer adjacent the acoustical core layer and the remainder of the sheet, including the core layer itself.

[0020]

[0020] As shown in FIG. 2, in one embodiment, the device may include (1) an unwinding unit, (2) an optional edge trim unit, (3) one or more tension rolls, (4) a positioning roll with optional cooling, (5) a heating or annealing unit, (6) an additional or second positioning roll with optional cooling, (7) a first layer pull roll for the first layer or skin layer, (8) a remainder pull roll for the remainder of the sheet, typically the core-skin bilayer, (9) one or more tension rolls for the first layer or skin layer, (10) one or more tension rolls for the remainder of the sheet, typically the core-skin bilayer, (11) a skin layer collecting unit, which may be a winder, a container with or without a nip system, or a granulator, and (12) a core-skin bilayer collecting unit, which may be a winder, a container with or without a nip system, or a granulator.

[0021]

[0021] The unwinding unit (1) may be motorised or non-motorised and ideally is capable of handling roll widths of, for example, up to 1.4m and roll weights of 500kg.

[0022]

[0022] The optional edge trim unit (2) can trim either one or both sides of the sheet along the length of the sheet as required before the sheet is transferred to the heating unit (5) to ensure a consistent width of the sheet, separate and collect only the required portion of the sheet, and prevent tearing from the edges. Such cases include, but are not limited to, trimming the beveled portion of the sheet, or trimming the edges of the sheet without the core layer. Generally, it is effective to trim at least about 25 mm from each edge with a fixed blade. This can be done before the roll is placed in the unwinding unit (1) or at any point between the unwinding unit (1) and the heating unit (5).

[0023]

[0023] One or more tension rolls (3) are typically motorized to pull the sheet from the unwinding unit (1) and feed it into a heating or annealing unit (5). If the tension is not set properly to flatten the sheet as it passes through the tension rolls, the sheet may wrinkle across its width, causing uneven heating and processing problems.

[0024] A first positioning roll (4) with optional cooling follows the tension roll (3) and is positioned adjacent to the main heat energy source of the heating unit (5) or annealing unit (5) to position the sheet on the correct path and establish the proper level of tension before it reaches the heating unit (5). This roll has optional cooling capability to fine-tune the sheet temperature. This roll is usually not motorized.

[0025]

[0025] The heating unit (5) contacts one or both of the skin layers such that the interfacial bond energy between at least one of the skin layers and the core layer is low. This makes it easier to mechanically separate one of the skin layers from the remainder of the sheet when a pulling force is applied. The thermal energy source can be either a single or multiple heated rolls, or infrared heaters, or a combination of both, which can be placed on one or both sides of the sheet. For commercial operation, it is important that the mechanically separated interface of the sheet, i.e. the orientation angle shown in FIG. 3, is maintained and remains consistent throughout the operation, i.e., the first layer is the layer that is removed from the remainder of the sheet throughout the operation. If not, the layer collected in the first layer collecting unit may also include the remainder of the sheet, e.g. the core layer. Therefore, it may be preferable that the thermal energy to the sheet is mainly supplied through conduction by the heated rolls.

[0026] The temperature range of the thermal energy source, typically the sheet surface closest to the first or skin layer, can be from about 25°C to about 70°C, or 30°C to 65°C, or 35°C to about 60°C, or as described elsewhere herein. This can be measured with an IR thermometer at the exit of the heating unit. If the temperature of the sheet surface is too low, mechanical separation will not occur and the sheet may tear. If the temperature of the sheet surface is too high, the mechanical integrity of the sheet may be reduced, making stable operation of the mechanical separation process difficult. The annealing or heating unit (3) is preferably a motorized roller.

[0027]

[0027] In other embodiments, the temperature of the sheet surface closest to the thermal energy source, typically the first layer or skin layer, achieved by the annealing unit is at least about 25°C, or at least about 26°C, or at least 27°C, or at least 28°C, or at least 30°C, or at least 32°C, or at least 35°C, and up to about 70°C, or up to 65°C, or up to 60°C, or up to 55°C, or up to 50°C.

[0028]

[0028] The second positioning roll (6) with optional cooling is placed opposite the main heat energy source of the heating unit (5) or annealing unit to establish the proper level of tension in the sheet by placing the sheet on the correct path before it reaches the separation point. This roll has optional cooling capacity to fine-tune the sheet temperature. The optional cooling second positioning roll (6) can be a spreader roll designed to remove wrinkles in the sheet by surface action in the width direction, so that when the sheet reaches the separation point, it is wrinkle-free and can be separated cleanly. This roll is usually not motorized.

[0029] The multilayer sheet is then mechanically separated between a first layer pull roll (7) for the first layer or skin layer and a remainder pull roll (8) for the remainder or core-skin bilayer. The first layer pull roll (7) for the skin layer is downstream of the second positioning roll for separation (6) and mechanically separates the skin layer from the remainder of the sheet. The remainder pull roll (8) for the core-skin bilayer is also downstream of the second positioning roll for separation (6) and the heating or annealing unit (5) and removes the remainder, i.e. the core-skin bilayer.

[0030]

[0030] For commercial operation, it is important that the interface or orientation angle of the mechanically separated sheets is maintained and remains consistent throughout the operation, i.e., the first layer is the layer that is removed from the remainder of the sheets during continuous operation, as explained in Figure 3. Otherwise, the layer collected in the first layer collection unit may also include the remainder of the sheets, e.g., the core layer.

[0031]

[0031] As shown in Figure 3, according to the present invention, angle α is the angle defined by the first layer and the multilayer sheet at the separation point after the sheet leaves the second positioning roll. Angle β is the angle defined by the multilayer sheet and the remaining part of the multilayer sheet at the separation point after the sheet leaves the second positioning roll. Also shown in Figure 3 is angle γ defined by the first layer and the remaining part of the multilayer sheet after the separation point. As shown in the figure, the sum of the three angles, α + β + γ, is 360°.

[0032]

[0032] According to the invention, it is important that the angle α is equal to or smaller than the angle β, in particular the latter, and that such a condition is maintained throughout the entire running period of the continuous sheet separating operation. Usually, separators are designed so that the angle γ is less than or equal to 180° and greater than or equal to 30° throughout the entire running period of the continuous sheet separating operation.

[0033]

[0033] Therefore, according to the present invention, the angle α may be, for example, about 30° to about 150°, or about 35° to about 160°, or about 40° to about 165°. Furthermore, the angle β may be, for example, about 90° to about 180°, or about 95° to about 150°, or 100° to 120°. Similarly, the angle γ may be, for example, about 30° to about 180°, or 45° to 150°, or 50° to 120°.

[0034] In another aspect, the angles according to the present invention are as follows, where delta is β minus α: γ=180°;α=60°;β=120° Δ60° γ=150°;α=90°;β=120° Δ30° γ=120°;α=90°;β=150° Δ60° γ=100°;α=80°;β=180° Δ100°.

[0035]

[0035] In order to minimize wrinkling of the sheet after mechanical separation, the distance between the first pulling roll (7) for the skin layer and the remaining pulling roll (8) for the core-skin bilayer, defined as the distance between the centers of the two rolls (7) and (8), may be, for example, less than 50% of the width of the sheet to be processed. This value is defined as ψ. It may be more desirable if ψ is less than 30%, or less than 20%, or less than 15%.

[0036]

[0036] Furthermore, the first pulling roll (7) for the skin layer and the remainder pulling roll (8) may be spreader rolls to prevent wrinkles from forming in the mechanically separated layers.

[0037]

[0037] By "spreader roll" we mean a roll designed to remove wrinkles by surface action in the cross direction.

[0038]

[0038] To assist in driving the entire mechanical separation process and stably transport the separated first or skin layer and residual portion or core-skin bilayer to the skin layer collection unit (11) and the core-skin bilayer collection unit (12), respectively, the skin layer tension roll (9)(s) is preferably motorized synchronously with the first pull roll (7) for the skin layer, in the same way that the core-skin bilayer tension roll (10)(s) is preferably motorized synchronously with the residual portion pull roll (8) for the core-skin bilayer.

[0039] The skin layer collection unit (11) can be either a power winder, a granulator, or a container. This is where the recovered skin layers are collected for reuse in extrusion. Alternatively, the skin layers can simply be collected in a container or the like for further processing, with or without a nip system to steadily feed the sheet into the container.

[0040] The core-skin bilayer collection unit (12) can also be either a powered winder, or a pelletizer, or a container. The collected core-skin bilayer can be reused in extrusion, further mechanically processed, or transferred for use in chemical recycling. Similarly, the core-skin bilayer can simply be collected in a container or the like for further processing, with or without a nip system to steadily feed the sheet into the container.

[0041]

[0041] The total thickness range of sheets that can be processed with the device disclosed in the present invention is typically from about 0.254 mm to about 5.080 mm, or from 0.508 to 2.540 mm, or from 0.762 to 1.270 mm.

[0042] The operating speed at which such mechanical separation takes place on the device disclosed in the present invention may be, for example, about 2 to about 20 m / min, or 5 to 10 m / min, based on the unwinding speed of the sheet. Both pull rolls operate at a speed 1.1 to 2.5 times the unwinding speed. That is, the operating speed at the separation point is 2.2 to 50 m / min, or 5.5 to 25 m / min.

[0043] It is noted that in a multilayer poly(vinyl acetal) sheet, the surface of the first layer that was in contact with the remainder of the multilayer sheet is smoother than the outer surface of the multilayer sheet. Subsequent embossing and / or melt fracture occurs on the outer surface of the multilayer sheet as the sheet exits the extruder die. Thus, the present invention also relates to a sheet that exhibits a rough surface on its outer surface, e.g., due to melt fracture, and a smoother surface on what was the inner surface of the sheet during extrusion, since it was not embossed or subjected to melt fracture, and a method for making the same.

[0044]

[0044] Referring again to FIG. 3, the first skin layer is a film or sheet of interest that exhibits melt fracture on the surface facing angle α, while having a smooth surface on the surface facing angle γ.

[0045]

[0045] US Patent Application Publication No. 2008 / 0254302, the relevant disclosure of which is incorporated herein by reference, describes a multi-layer polymer interlayer having a melt-fractured surface. A particular problem encountered with multi-layer interlayers can occur during the lamination stage of processing. Traditionally, single-layer interlayers have been roller embossed to provide a texture that facilitates degassing, but a three-layer interlayer with a relatively soft inner layer between two relatively hard layers, such as some acoustic interlayers, creates optical distortions when the embossing of the outer interlayer surface transfers to the softer inner layer. EP Patent Application Publication No. 0710545 details this problem and warns against embossing the outer layer of a three-layer interlayer too deeply.

[0046]

[0046] Multi-layer interlayers may be formed having a surface topography that is formed by controlling the melt fracture that occurs at the exposed surfaces of the interlayer or individual layers of the multi-layer interlayer during formation of the interlayer.

[0047]

[0047] As used herein, the terms "multilayer" and "multi-layer" refer to an interlayer having two or more layers, and multilayer and multi-layer may be used interchangeably. The layers of the interlayer are generally produced by mixing a polymeric resin, such as poly(vinyl butyral), with one or more plasticizers and melt processing the mixture into a sheet by any applicable process or method known to those skilled in the art, including but not limited to extrusion, where the layers are bonded by processes such as coextrusion and lamination. Other additional components may be optionally added for various other purposes. After the interlayer sheet is formed, it is typically collected and rolled for transportation and storage, as described below, and for later use in multiple layer glass panels.

[0048]

[0048] A multi-layer interlayer, such as an interlayer having two or more layers (such as a three-layer interlayer having three layers), can include at least one soft layer and at least one hard layer. The soft layer is often the inner or core layer of an interlayer having at least three layers. To better understand the present invention, some terms used throughout this application are explained. As used herein, the terms "polymer interlayer sheet", "interlayer", "polymer layer", and "polymer melt sheet" may generally refer to a single layer sheet or a multi-layer interlayer.

[0049]

[0049] A "monolayer sheet", as the name suggests, is a single polymer layer extruded as one layer. A multilayer interlayer, on the other hand, may include multiple layers, including layers that are extruded separately, coextruded, or any combination of separate and coextruded layers. Thus, a multilayer interlayer may include, for example: two or more monolayer sheets bonded together ("multilayer sheet"); two or more layers coextruded together ("coextruded sheet"); two or more coextruded sheets bonded together; a combination of at least one monolayer sheet and at least one coextruded sheet; a combination of a monolayer sheet and a multilayer sheet; a combination of at least one multilayer sheet and at least one coextruded sheet.

[0050]

[0050] In various embodiments of the present disclosure, as described in more detail below, a multilayer interlayer includes at least two polymer layers (e.g., monolayers or multilayers coextruded and / or laminated together) disposed in direct contact with one another, each layer including a polymer resin. As used herein for a multilayer interlayer having at least three layers, "skin layer" generally refers to the outer layer of the interlayer, and "core layer" generally refers to the inner layer. Thus, one exemplary embodiment would be skin layer / / core layer / / skin layer. In a multilayer interlayer having a skin layer / / core layer / / skin layer configuration, in some embodiments, the skin layer may be harder and the core layer may be softer, while in other embodiments, the skin layer may be softer and the core layer may be harder. However, it should be noted that further embodiments include an interlayer having only two layers, or an interlayer having three or more layers (e.g., 4, 5, 6, or up to 10 or more individual layers). Additionally, any multilayer interlayer utilized can be varied by manipulating the composition, thickness, or position, etc., of the layers.

[0051] For example, in one three-layer polymer interlayer sheet, the two hard (or outer or skin) layers may comprise poly(vinyl butyral) ("PVB") resins containing a plasticizer or mixture of plasticizers, while the softer (inner or core) layer may comprise the same or different PVB resins, or different thermoplastic materials containing the same or different plasticizers and / or mixtures of plasticizers. Thus, it is contemplated that the hard or skin layers and the soft or core layers of a multi-layer interlayer sheet may be composed of the same or different thermoplastic materials, and the same or different plasticizer(s). If desired, either or both layers may contain additional additives known in the art.

[0052]

[0052] One type of multi-layer interlayer that utilizes a softer inner layer is a multi-layer acoustic type interlayer. As disclosed herein, an acoustic interlayer comprises multiple layers, and in a preferred embodiment has a relatively soft layer sandwiched between two relatively hard layers. The resulting three-layer interlayer can generally be used directly in a lamination process in place of a conventional single layer interlayer with little or no modification to the lamination process.

[0053]

[0053] Although the invention is described throughout this specification as applicable to such acoustic interlayers, those skilled in the art will understand that the invention can also include multi-layer interlayers, such as three-layer interlayers, having an inner polymer layer that is softer than the outer layers between which it is disposed, including non-acoustic multi-layer interlayers.

[0054] The present invention also includes multilayer sheets comprising two different polymers, for example poly(vinyl butyral) and sulfopolyester.

[0055]

[0055] Degassing of the multilayer interlayer can be easily achieved without embossing by deliberately introducing melt fracture into the outer layers of the multilayer interlayer. Melt fracture is typically controlled by forming the layers through a rectangular sheet die opening formed by a land that is at a lower temperature than the bulk of the melt being extruded. This is accomplished by moving a conditioning liquid through a channel just below the surface of the land. Melt fracture can be further controlled at the outer surfaces of one or both of the outer layers of a multi-layer intermediate layer by controlling other processing parameters of the extruded layers (see U.S. Pat. No. 5,455,103; U.S. Pat. Nos. 6,077,374, 5,425,977, 4,281,980, and 4,575,540, and "Polymer Processing Instabilities: Control and Understanding," edited by Savvas Hatzikiriakos and Kalman Migler, CRC Press 2004, ISBN 0824753860, the relevant disclosures of which are incorporated herein by reference).

[0056] Thus, melt fracture can be induced on one side of a polymer layer, for example, by extruding the polymer onto a die roll, or on both sides of a polymer layer, for example, by extruding the polymer directly into air and then into a cooling bath.

[0057]

[0057] Thus, one or both sides of an outer polymer layer can be produced using this controlled melt fracture to produce a polymer layer having a desired "roughness" or "Rz." Rz is a measure of the surface topography of a polymer layer, indicating the departure of the surface from planarity.

[0058]

[0058] As used herein, the surface roughness, or the height of a particular peak on a rough surface from an imaginary plane of the flattened polymer interlayer sheet, is the Rz value of the surface. The surface roughness, or Rz, of the surfaces of the polymer interlayer sheets described in this application is measured by a 10-point average roughness according to DIN ES ISO-4287 of the International Organization for Standardization and ASME B46.1 of the American Society of Mechanical Engineers, and is expressed in microns (μ). Under these scales, Rz is calculated as the arithmetic average value of the single roughness depths Rzi (i.e., the vertical distance between the highest peak and the deepest valley within the sampling length) of successive sampling lengths: Rz = -x(Rz1 + Rz2 + ... + RzN)

[0059] The surface roughness Rz values ​​reported were measured using a model S8P Perthometer from Mahr Corp., Cincinnati, Ohio.

[0059]

[0060] According to the invention, a smooth surface with an Rz of about 0 to about 10, or 0.5 to 8, or 1 to 7 may be achieved on one side, while a rough surface will typically exhibit a value of about 10 to about 150, or 15 to 120, or 20 to 100. Alternatively, a smooth surface may have an Rz of at least 0.01, or at least 0.1, or at least 0.2, or at least 0.5, up to about 10, or up to 9, or up to 8, or up to 7. Similarly, a rough surface may exhibit an Rz of up to about 150, or up to 125, or up to 120, or up to 100, or up to 90, or up to 80, or up to 70, or up to 60, or up to 50, or at least 10, or at least 12, or at least 15, or at least 18, or at least 20, or at least 30.

[0060]

[0061] Thus, a multi-layer interlayer can be produced, for example, without embossing, in which case the outer surface of the interlayer imparted by melt fracture has an Rz value, for example, of 20 to 60, or 25 to 50, or as described elsewhere herein. The two outer surfaces can have the same Rz value, or different values, or only one of the two outer surfaces can have the specified Rz value.

[0061]

[0062] Multi-layer interlayers can also be produced, for example, using embossing, where the outer surface of the interlayer imparted by melt fracture has an Rz value, for example, of 20 to 120, or 25 to 100, or as described elsewhere herein.

[0062]

[0063] Extruded interlayers formed from plasticized, lightly crosslinked PVB resin can be prepared using systems known to those skilled in the art by extruding through a conventional sheet die having water-cooled die lips, i.e., by forcing the molten polymer into a horizontally long, vertically narrow die opening that substantially matches the length and width of the sheet to be formed therein. It is hypothesized that the more rubbery the polymer, the greater its tendency to contract itself as it exits the extrusion die to provide a given surface roughness.

[0063]

[0064] For example, the multi-layer interlayer can be coextruded using a multiple manifold coextrusion device such as that disclosed in US Patent Application Publication No. 2008 / 0254302, the relevant disclosure of which is incorporated herein by reference. Such a device has a first die manifold, a second die manifold, and a third die manifold. The device operates by simultaneously extruding the polymer melt from each manifold toward the extrusion orifice where the multi-layer interlayer is extruded as a composite of three individual polymer layers. The thickness of the layers can be varied by adjusting the distance between the die lips of the extrusion orifice. Melt fracture can be controlled by controlling the composition of the melt, the temperature of the die lips or lands of the extrusion orifice, or by controlling the rate and manner of cooling of the extruded interlayer, for example, by immersion in a cooling bath immediately after extrusion. In accordance with the present invention, the separation techniques described herein can be used to obtain a desired film having a rough surface and a smooth surface on opposite sides.

[0064]

[0065] The present invention also relates to a poly(vinyl acetal) film that can be produced by a process comprising the steps of forming at least a first polymer melt comprising poly(vinyl butyral) and a second polymer melt comprising a sulfopolyester, coextruding at least the first polymer melt and the second polymer melt to form a multilayer interlayer comprising a first layer and a remainder of the multilayer sheet comprising the second layer, the multilayer sheet having a surface roughness imparted to its outer surface by melt fracture during coextrusion, and then separating the first layer from the remainder of the multilayer interlayer sheet by dissolving the sulfopolyester.

[0065]

[0066] When the sulfopolyester is extruded in this manner with the poly(vinyl acetal) layer, the sulfopolyester can be dissolved or washed off with water or other solvent. Sulfopolyesters suitable for use in accordance with the present invention include those having a glass transition temperature (Tg) of at least 25°C, such as, for example, (A) those having the residues of one or more dicarboxylic acids; (B) from about 4 to about 40 mole percent, based on the total repeat units, of the residues of at least one sulfomonomer having two functional groups attached to an aromatic or alicyclic ring and one or more sulfonate groups, where the functional groups are hydroxyl, carboxyl, or combinations thereof; (C) at least 25 mole percent, based on the total diol residues, of the residues of a diol having the structure H(OCH2CH2) n (D) from 0 to about 25 mole %, based on the total repeat units, of residues of branched monomers having three or more functional groups, the functional groups being hydroxyl, carboxyl, or combinations thereof. The sulfopolyester may optionally include a water-dispersible polymer blended with the sulfopolyester. Other suitable water-dispersible sulfopolyesters useful in accordance with the present invention include those disclosed and claimed in U.S. Patent Nos. 6,171,685; 5,543,488; 5,853,701; 4,304,901; 6,211,309; 5,570,605; 6,428,900, and 3,779,993, the relevant disclosures of which are incorporated herein by reference.

[0066]

[0067] The described mechanical separation device can be started as follows: [a] Cut the three-ply interlayer sheets diagonally, one by one, in both directions from the center of their leading edge to create an arrow-shaped leading edge of the sheets; [b] Manually peel one skin layer from the three-ply interlayer sheet at the arrow-shaped leading edge and continue the separation of the sheets for about 25 cm; [c] Manually press the separated first skin layer and core-skin bilayer firmly against the skin layer pull roll (7) and core-skin bilayer pull roll (8), respectively, very slowly, e.g. , jog the machine at a slow speed slower than 1.0 m / min to start threading up; [d] thread up the skin layer through the skin layer pull roll (7) to the skin layer tension roll (9); [e] thread up the core-skin bilayer through the core-skin bilayer pull roll (8) to the core-skin bilayer tension roll (10); [f] jog all motorized rolls to ensure a stable process is established; [g] increase speed to the target to reach steady state.

[0067]

[0068] Another approach to initiating mechanical separation is to attach a "preliner" to the skin layer of the multilayer sheet. The preliner is a piece of sheet, preferably of the same composition and width as the skin layer material, long enough to reach the pull roll and allow the pull roll to exert a pulling force as it is guided through the separation unit. In the case of a poly(vinyl butyral) interlayer, the preliner can be attached to the skin layer material by melting or gluing. Two preliners, one for each skin layer, can be attached to the multilayer sheet by using a heat sealing device that applies the appropriate amount of heat and pressure to the stack of preliners, multilayer interlayers, and preliners. Applying too much heat or pressure will inhibit separation. Applying too little heat or pressure will cause the preliner to peel away from the skin layer surface and initiation to fail.

[0068]

[0069] As an alternative to using heat and pressure to fuse the preliner and skin layer surfaces, a suitable solvent can be applied to the surface of the preliner or multilayer skin and the solvent allowed to evaporate or diffuse into the material before the two surfaces are pressed together. For this method to be successful, the preliner must be attached close enough to the edge of the multilayer sheet. Other means and methods can also be applied to initiate the separation process, for example, a vacuum can be used to attach a towing lever to the skin surface with sufficient force to successfully initiate a continuous process.

[0069]

[0070] It will be appreciated that once at steady state, the multi-layer interlayer sheet moves through the device as follows: the sheet is unwound from unwinding unit 1 and optional edge trim unit 2, then passes through tension roll 3 at ambient temperature before reaching first positioning roll 4. First positioning roll 4, with optional cooling, can be cooled, for example, to about ambient temperature, or the temperature of tap water, or about 10°C to about 30°C, or 15°C to 30°C, or 20°C to 25°C, to bring the temperature of the surface of the sheet to, for example, about 15°C to about 30°C, or 20°C to 25°C.

[0070]

[0071] The sheet is then contacted with a heating unit 5, preferably a heated roll, which heats the surface of the sheet closest to the thermal energy source to a temperature of from about 35° C. to about 80° C., or from 43° C. to 75° C., or from 45° C. to 65° C., or as described elsewhere herein.

[0071]

[0072] After the sheet has been heated by the heating unit 5, it is conveyed from the first positioning roll to a second positioning roll (6) with optional cooling, located on the opposite side of the heating unit (5) or the main heat energy source of the heating unit (5). The second positioning roll 6 can be cooled to a temperature that brings the temperature of the surface of the sheet to about 5°C to about 40°C, or 10°C to 30°C, or 12°C to 35°C, for example as described above. Alternatively, the surface of the sheet in contact with the second positioning roll 6 may be cooled to a temperature of at least 5°C, or at least 10°C, or at least 12°C, or at least 15°C, up to about 40°C, or up to 35°C, or up to 30°C.

[0072]

[0073] After the sheet passes over the second positioning roll 6, the multi-layer sheet is mechanically separated by pulling the first layer by the first skin layer pull roll 7 and the remainder of the sheet in the direction described above by the remainder pull roll 8. As noted above, this mechanical separation is initiated during start-up, and thereafter the method and device of the present invention ensures that the two layers remain cleanly separated during continuous operation.

[0073]

[0074] As mentioned above, to minimize wrinkling of the sheet after mechanical separation, in one embodiment the distance between the first layer skin layer pull roll 7 and the remainder core-skin bilayer pull roll 8, defined as the distance between the centers of the two rolls 7 and 8, is less than about 30% of the width of the sheet being processed, which may be more desirable if the number is less than 25%, or less than 20%, or less than 15%.

[0074]

[0075] As noted above, in important aspects, the multi-layer interlayer sheet includes a multi-layer PVB interlayer having, for example, a skin / core / skin cross-section. Although a particular PVB interlayer has been described, a variety of interlayer materials can be used.

[0075]

[0076] When the intermediate layer comprises polyvinyl butyral (PVB), the PVB resin can be produced by the known acetalization process in which polyvinyl alcohol ("PVOH") is reacted with butyraldehyde in the presence of an acid catalyst, and the resin is isolated, stabilized, and dried. Such acetalization processes are disclosed, for example, in U.S. Pat. Nos. 2,282,057 and 2,282,026, in Vinyl Acetal polymers in Encyclopedia of Polymer Science & Technology, 3rd Edition, Vol. 8, pp. 381-399 (2003) by BEWade, the entire disclosure of which is incorporated herein by reference. This resin is commercially available in various forms, for example, as Butvar® resin from Solutia Inc., a wholly owned subsidiary of Eastman Chemical Company.

[0076]

[0077] As used herein, the residual hydroxyl content in PVB (calculated as weight percent vinyl alcohol or weight percent PVOH) refers to the amount of hydroxyl groups remaining on the polymer chain after processing is complete. For example, PVB can be produced by hydrolyzing poly(vinyl acetate) to poly(vinyl alcohol (PVOH)) and then reacting the PVOH with butyraldehyde. In the process of hydrolyzing poly(vinyl acetate), not all of the acetate side groups are typically converted to hydroxyl groups. Furthermore, in the reaction with butyraldehyde, not all of the hydroxyl groups are typically converted to acetal groups. Thus, any finished PVB resin will typically have residual acetate groups (as vinyl acetate groups) and residual hydroxyl groups (as vinyl hydroxyl groups) as side groups on the polymer chain. As used herein, the residual hydroxyl content and residual acetate content are measured on a weight percent (wt%) basis according to ASTM D1396.

[0077]

[0078] The PVB resins of the present disclosure typically have a molecular weight of greater than 50,000, or less than 500,000, or from about 50,000 to about 500,000 daltons, or from about 70,000 to about 500,000 daltons, or from about 100,000 to about 425,000 daltons, as measured by size exclusion chromatography using low angle laser light scattering. As used herein, the term "molecular weight" means weight average molecular weight.

[0078]

[0079] Various adhesion control agents ("ACA") can be used in the interlayer of the present disclosure to control adhesion of the interlayer sheet to glass. In various embodiments of the interlayer of the present disclosure, the interlayer can include from about 0.003 to about 0.15 parts ACA per 100 parts resin; from about 0.01 to about 0.10 parts ACA per 100 parts resin; from about 0.01 to about 0.04 parts ACA per 100 parts resin. Such ACAs include, but are not limited to, ACAs disclosed in U.S. Pat. No. 5,728,472, the disclosure of which is incorporated herein by reference in its entirety, residual sodium acetate, potassium acetate, magnesium bis(2-ethylbutyrate), and / or magnesium bis(2-ethylhexanoate).

[0079]

[0080] Other additives may also be incorporated into the interlayer to improve the performance of the final product or to impart specific additional properties to the interlayer. Such additives include, but are not limited to, dyes, pigments, stabilizers (e.g., UV stabilizers), antioxidants, antiblocking agents, flame retardants, IR absorbers or blockers (e.g., indium tin oxide, antimony tin oxide, lanthanum hexaboride (LaB6), and cesium tungsten oxide), processing aids, flow additives, lubricants, impact modifiers, nucleating agents, heat stabilizers, UV absorbers, dispersants, surfactants, chelating agents, coupling agents, adhesives, primers, toughening additives, and other additives known to those skilled in the art, such as fillers.

[0080]

[0081] Although the described embodiment refers to the polymer resin as PVB, one skilled in the art will understand that the polymer can be any polymer suitable for use in a multi-layer panel. Exemplary polymers include, but are not limited to, polyvinyl acetal (PVA) (such as poly(vinyl butyral) (PVB) or isomeric poly(vinyl isobutyral) (PVisoB)), polyurethane (PU), poly(ethylene-co-vinyl acetate) (EVA), polyvinyl chloride (PVC), poly(vinyl chloride-co-methacrylate), polyethylene, polyolefins, ethylene acrylic acid ester copolymers, poly(ethylene-co-butyl acrylate), silicone elastomers, epoxy resins, acid copolymers such as ethylene / carboxylic acid copolymers and ionomers thereof derived from any of the above possible thermoplastic resins, combinations of the above, and the like. PVB and its isomeric polymer PVisoB, polyvinyl chloride, and polyurethanes are particularly useful polymers for the interlayer in general, with PVB (and its isomeric polymers) being particularly preferred.

[0081]

[0082] In further embodiments, the interlayer may be a multi-layer interlayer. For example, the multi-layer interlayer may be composed of PVB / / PVisoB / / PVB. Other examples include PVB / / PVC / / PVB or PVB / / PU / / PVB. Further examples include PVC / / PVB / / PVC or PU / / PVB / / PU. Alternatively, the skin layers and core layer may all be PVB using the same or different starting PVB resins.

[0082]

[0083] In one embodiment, the first or skin layer of the multilayer interlayer sheet comprises a PVB polymer having a Tg of, for example, from about 20° C. to about 45° C., or from 25° C. to 40° C., or from 28° C. to 35° C. Alternatively, the Tg of the poly(vinyl butyral) can be at least about 20° C., or at least 25° C., or at least 28° C., up to about 45° C., or up to 40° C., or up to 35° C.

[0083]

[0084] In one embodiment, the Tg of the layer adjacent to the first layer may be at least 12° C. lower, or at least 15° C. lower, or at least 20° C. lower, or at least 30° C. lower than the Tg of the first layer.

[0084]

[0085] Unless otherwise indicated, all numbers expressing quantities of ingredients, properties such as molecular weights, reaction conditions, and the like used in the specification and claims should be understood in all instances as modified by the term "about." Thus, unless otherwise indicated, the numerical parameters set forth in the following specification and appended claims are approximations that may vary depending on the desired properties sought to be obtained by the present invention. In any event, each numerical parameter should be construed in light of at least the number of reported significant digits and by applying ordinary rounding techniques. Moreover, ranges set forth in the present disclosure and claims are specifically intended to include the entire range, not just the endpoint(s). For example, a range set forth as 0-10 is intended to disclose all integers between 0 and 10, e.g., 1, 2, 3, 4, etc., all fractions between 0 and 10, e.g., 1.5, 2.3, 4.57, 6.1113, etc., as well as the endpoints of 0 and 10.

[0085]

[0086] Notwithstanding that the numerical ranges and parameters setting forth the broad scope of the invention are approximations, the numerical values ​​set forth in the specific examples are intended to be reported precisely given the measuring techniques used, however, any numerical value inherently contains certain errors necessarily resulting from the standard deviation found in their respective testing measurements.

[0086]

[0087] It should be understood that the reference to one or more process steps does not exclude the presence of additional process steps before or after any combination of the recited steps or any intervening process steps between the steps expressly identified. Furthermore, the designations of process steps, components, or other aspects of the information disclosed or claimed in the application by letters, numbers, or the like are convenient means of identifying separate activities or components, and unless otherwise noted, the recited letters can be arranged in any order.

[0087]

[0088] As used herein, the singular forms "a," "an," and "the" include plural referents unless the context clearly dictates otherwise. For example, n References to alcohol equivalents include multiple types of C n alcohol equivalents. Thus, the use of language such as "at least one" or "at least some" in one place is not intended to imply that other uses of "a," "an," and "the" exclude multiple referents, unless the context clearly dictates otherwise. Similarly, the use of language such as "at least some" in one place is not intended to imply that the absence of such language in other places indicates that "all" is intended, unless the context clearly dictates otherwise.

[0088]

[0089] As used herein, the term "and / or," when used in a list of two or more items, means that any one of the listed items can be used alone, or any combination of two or more of the listed items can be used. For example, if a composition is described as containing components A, B, and / or C, the composition can contain only A, only B, only C, a combination of A and B, a combination of A and C, a combination of B and C, or a combination of A, B, and C.

[0089]

[0090] The present invention can be further illustrated by the following examples of embodiments thereof, although it will be understood that these examples are included for illustrative purposes only and are not intended to limit the scope of the invention unless specifically stated. EXAMPLES

[0090] Example 1

[0091] A mechanical separation device as shown in FIG. 2 was operated to mechanically separate the skin layers and core-skin bilayer of a 1.2 m wide, 0.813 mm thick flat 3-ply PVB interlayer sheet across the width of the sheet under the following conditions: Rewind speed: 12m / min First skin pull roll speed (speed at separation): 25 m / min Edge Trimming: None Sheet temperature at the exit of the annealing unit: 38℃ ψ [distance between two pull rolls / sheet width]: 15% α=60° β=120° γ=180°

[0092] The operation was stable with no sheet breakage. The separation interface remained consistent and there were no wrinkles in the skin layer.

[0091] Example 2

[0093] The mechanical separation device shown in FIG. 2 was operated to mechanically separate the skin layers and the core-skin bilayer of a wedge three-ply PVB interlayer sheet having a width of 1.2 m and a thickness of 0.838-1.143 mm across the width of the sheet under the following conditions: Rewind speed: 5m / min First skin pull roll speed (separation speed): 10 m / min Edge trimming: Yes Sheet temperature at the exit of the annealing unit: 35℃ ψ [distance between two pull rolls / sheet width]: 30% α=90° β=120° γ=150°

[0094] The operation was stable with no sheet breakage. The separation interface remained consistent and there were no wrinkles in the skin layer.

[0092] Example 3

[0095] A mechanical separation device as shown in Figure 2 was operated to mechanically separate the skin layer and the core-skin bilayer of a flat 3-ply PVB interlayer sheet 1.2 m wide and 0.813 mm thick, containing a band with a gradient width of 24 cm in one of the skins, across the width of the sheet under the following conditions: Rewind speed: 5m / min First skin pull roll speed (separation speed): 10 m / min Edge Trimming: None Sheet temperature at the exit of the annealing unit: 35℃ ψ [distance between two pull rolls / sheet width]: 30% α=90° β=150° γ=120°

[0096] The operation was stable with no sheet breakage. The separation interface remained consistent and there were no wrinkles in the skin layer.

[0093] Example 4

[0097] A mechanical separation device as shown in FIG. 2 was operated to mechanically separate the skin layers and core-skin bilayer of a 1.2 m wide, 0.813 mm thick flat 3-ply PVB interlayer sheet across the width of the sheet under the following conditions: Rewind speed: 10m / min First skin pull roll speed (separation speed): 24 m / min Edge Trimming: None Sheet temperature at the exit of the annealing unit: 45℃ ψ [distance between two pull rolls / sheet width]: 15% α=80° β=180° γ=100°

[0098] The operation was stable with no sheet breakage. The separation interface remained consistent and there were no wrinkles in the skin layer.

[0094] Example 5

[0099] Using a mechanical separation device as shown in FIG. 2, as before, the skin layers and core-skin bilayer of a flat 3-ply PVB interlayer sheet, 1.2 m wide and 0.813 mm thick, were mechanically separated across the width of the sheet under the following conditions: Rewind speed: 2m / min First skin pull roll speed (separation speed): 5m / min Edge trimming: Yes Sheet temperature at the exit of the annealing unit: 40℃ y [distance between two pull rolls / sheet width]: 15% In this example, we have changed the angle such that the previous angle, described as α, is now greater than the previous angle, described as β, according to the following: α=120° β=60° γ=180°

[0100] The operation was stable, but the angle defined as α was greater than the angle defined as β, so the skin layer entered the bilayer collection unit described above.

[0095] Example 6

[0101] A mechanical separation device as shown in FIG. 2 was operated to mechanically separate the skin layers and core-skin bilayer of a 1.4 m wide, 0.813 mm thick flat 3-ply PVB interlayer sheet across the width of the sheet under the following conditions: Rewind speed: 2m / min First skin pull roll speed (separation speed): 5m / min Edge trimming: Yes Sheet temperature at the exit of the annealing unit: 38℃ ψ [distance between two pull rolls / sheet width]: 15% In this example, we have changed the angle such that the previous angle, described as α, is now greater than the previous angle, described as β, according to the following: α=120° β=90° γ=150°

[0102] Attempting to correctly guide the skin layers into the skin layer collection unit resulted in unstable operation with the core layer frequently moving to the side. It was not possible to achieve a steady state where the first skin layer always entered the desired skin layer collection unit.

[0096] Example 7

[0103] A mechanical separation device as shown in FIG. 2 was operated to mechanically separate the skin layers and core-skin bilayer of a 1.2 m wide, 0.813 mm thick flat 3-ply PVB interlayer sheet across the width of the sheet under the following conditions: Rewind speed: 2m / min First skin pull roll speed (separation speed): 5m / min Edge trimming: Yes Sheet temperature at the exit of the annealing unit: 20℃ ψ [distance between two pull rolls / sheet width]: 15% α=90° β=120° γ=150°

[0104] Due to the low temperature, the operation was not very stable, as the sheet started to tear sporadically from the edges and the core layer frequently moved sideways.

[0097] Example 8

[0105] A mechanical separation device as shown in FIG. 2 was operated to mechanically separate the skin layers and core-skin bilayer of a flat 3-ply PVB interlayer sheet having a width of 0.4 m and a thickness of 0.813 mm across the width of the sheet under the following conditions: Rewind speed: 2m / min First skin pull roll speed (separation speed): 5m / min Edge Trimming: None Sheet temperature at the exit of the annealing unit: 38℃ ψ [distance between two pull rolls / sheet width]: 70% α=90° β=120° γ=150°

[0106] Although the operation could be established, due to the high ψ value, the separated first skin had many wrinkles when it was sent to the skin layer collecting unit.

[0098] Example 9

[0107] A mechanical separation device as shown in FIG. 2 was operated to mechanically separate the skin layers and core-skin bilayer of a 1.2 m wide, 0.813 mm thick flat 3-ply PVB interlayer sheet across the width of the sheet under the following conditions: Rewind speed: 2m / min First skin pull roll speed (separation speed): 5m / min Edge trimming: Yes Sheet temperature at the exit of the annealing unit: 75℃ ψ [distance between two pull rolls / sheet width]: 30% α=90° β=120° γ=150°

[0108] Due to higher than optimal temperatures, frequent sheet tears occurred and operation was unstable; it was impossible to reach a steady state.

[0099] [Table 1]

[0100] Examples 10a to 10c. Method for producing a sheet having a smooth surface and a rough surface.

[0101] Example 10a.

[0109] The multi-layer PVB sheets with embossed skins were separated by hand and within 1 hour of separation gave the following properties: Rough surface: Rz=40.8 Smooth (inner) surface: Rz=1.2 Example 10b.

[0110] Multilayer PVB sheets having skins that were melt fractured during extrusion were manually separated within one hour of separation and gave the following properties: Rough surface: Rz=14.6 Inside the separated skin: Rz=1.3 Example 10c.

[0111] Multilayer PVB sheets having skins that were melt fractured during extrusion were manually separated within one hour of separation and gave the following properties: Outer rough skin: Rz=64.9 Smooth inner surface: Rz=2.3

Claims

1. 1. A continuous process for separating a first layer from a remainder of a multi-layer interlayer sheet, comprising: a. heating the multi-layer sheet; and b. thereafter, separating the first layer of the multi-layer interlayer sheet from the remainder by pulling the first layer and the remainder of the multi-layer interlayer sheet in different directions; A process wherein during a continuous process, an angle α defined by the first layer and the multilayer sheet at the separation point is less than or equal to an angle β defined by the multilayer sheet at the separation point and the remainder of the multilayer sheet.

2. 1. A continuous process for separating a first layer from a remainder of a multi-layer interlayer sheet, comprising: a. heating the multi-layer sheet to a temperature of about 25° C. to about 70° C.; and b. thereafter, separating the first layer of the multi-layer interlayer sheet from the remaining portion by pulling the first layer and the remaining portion of the multi-layer interlayer sheet in different directions in an orientation; An angle α is defined by the first layer and the multilayer sheet at the separation point, an angle β is defined by the multilayer sheet at the separation point and the remainder of the multilayer sheet, and an angle γ is defined by the first layer and the remainder of the multilayer sheet at the separation point, and is determined by the following formula: β／α≧１ 30°≦γ≦180° α + β + γ = 360° Fulfilling A process in which the orientation is maintained during a continuous process.

3. 10. The continuous process of claim 1, wherein the multi-layer sheet comprises poly(vinyl acetal) and the multi-layer sheet is heated to a temperature of from about 25°C to about 70°C.

4. 2. The continuous process of claim 1 , wherein during the continuous process, angle α is less than angle β.

5. The process of any one of claims 1 to 4, wherein angle α is at least 50 degrees less than angle β.

6. The process of any one of claims 1 to 4, wherein angle α is about 30 degrees to about 75 degrees less than angle β.

7. The process of any of claims 1 to 4, wherein the first layer comprises a poly(vinyl butyral) polymer having a Tg of about 25°C to about 40°C.

8. The process according to any of claims 1 to 4, wherein the multilayer sheet is heated in step a) to a temperature of from 30°C to 70°C.

9. The process of any of claims 1 to 4, wherein at least a portion of the remainder of the multilayer sheet comprises a poly(vinyl butyral) polymer having a Tg at least 15°C lower than the Tg of the first layer.

10. In the separating step, the first layer is pulled by a first layer pull roll, and the remaining portion of the multi-layer interlayer sheet is pulled by a remaining portion pull roll; The process of any one of claims 1 to 4, wherein the distance between the first layer pull roll and the remainder pull roll is maintained at less than about 50% of the width of the sheet while separation is occurring.

11. The process of any one of claims 1 to 4, wherein the distance between the first layer pull roll and the remainder pull roll during separation is less than about 15% of the width of the sheet.

12. The process of any one of claims 1 to 4, wherein the multilayer sheet comprises a core layer having skin layers on each side.

13. The process of any one of claims 1 to 4, wherein a first end of the multi-layer sheet is thicker than a second end of the multi-layer sheet, the ends being defined in the machine direction.

14. The process of any one of claims 1 to 4, wherein the first layer comprises a first skin layer, the first skin layer being thicker than the other skin layer.

15. The process of any one of claims 1 to 4, wherein the first layer comprises a first skin layer, the first skin layer being thinner than the other skin layer.

16. The process of any of claims 1 to 4, wherein the first end of the multi-layer sheet is thicker than the second end of the multi-layer sheet.

Images