PROCESS FOR PRODUCTION OF EMBOSSED FILMS BASED ON PLASTICIZED POLYVINYL ACETAL

Abstract

Polyvinyl acetal films with less blocking tendency and which allow for escape of gas during laminating to form laminated composities are prepared by a process for embossing a film comprising plasticized polyvinyl acetal with a roughness Rz on at least one surfaces of 20 to 100 μm by the steps of a. extruding of plasticised polyvinyl acetal to a film with a stochastic roughness of the surfaces of Rz=1 to 70 μm, b. embossing at least one surface of the film obtained in step a) with channels having a depth of 5-50 μm, a width of 10-200 μm and a pitch of 50-2500 μm, wherein c. the surface roughness of the elevations between the channels is at most 20% lower as obtained in step a).

Claims

1.-11. (canceled)

12. A process for embossing a film comprising plasticized polyvinyl acetal with a roughness Rz of 20 to 100 μm, on at least one surface comprising: a. extruding a plasticised polyvinyl acetal to a film with a stochastic roughness of the surfaces of Rz=1 to 70 μm, b. embossing at least one surface of the film obtained in step a) with channels having a depth of 5-50 μm, a width of 10-200 μm and a pitch of 50-2500 μm, wherein c. the surface roughness of the elevations between the channels is at most 20% lower as obtained in step a).

13. The process of claim 12, wherein the film is embossed with an embossing roller having a temperature of 80 to 200° C.

14. The process of claim 12, wherein the film is embossed with a line pressure of 10 to 400 N/mm.

15. The process of claim 13, wherein the film is embossed with a line pressure of 10 to 400 N/mm.

16. The process of claim 12, wherein the extrusion of the plasticized polyvinyl acetal film in step a) is performed under melt-fracture conditions.

17. The process of claim 16, wherein the extrusion under melt-fracture conditions is performed with an extrusion die having lip temperatures of 100-270° C.

18. The process of claim 16, wherein the extrusion under melt-fracture conditions is performed with a melt flow rate of 500-3500 kg/h.

19. The process of claim 12, wherein both surfaces of the embossed film have the same pitch of channels.

20. The process of claim 12, wherein both surfaces of the embossed film have a different pitch of channels.

21. The process of claim 12, wherein the channels on both surfaces of the film have an angle of 70-90° with respect to each other.

22. The process of claim 12, wherein the channels on at least one surface of the film have an angle of 5-45° to the direction of extrusion.

23. The process of claim 12, wherein the surfaces of the film are embossed in two distinct embossing steps.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0022] FIG. 1 illustrates one embodiment of an embossed plasticized polyvinyl acetal film of the invention.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0023] The stochastic surface pattern on the elevations between the channels are created during step a) and should remain during embossing step b) essentially as obtained during step a).

[0024] Preferably, the surface roughness of the elevations between the channels obtained in step b) is at most 10%, more preferably at most 5% lower as obtained in step a. At best, the surface roughness of the elevations between the channels obtained in step a) and step b) is (remains) identical. This can be achieved by an embossing tool which has no or no full contact with the film in the areas of the elevations.

[0025] The extrusion of the melt comprising plasticised polyvinyl acetal in step a) is preferably performed under melt fracture conditions with an extrusion die having lips whose temperature can be adjusted. Such an extrusion process is known to the person skilled in the art for example from EP 0 185 863 B1.

[0026] The stochastic surface pattern on the elevations between the channels may be the same or different on the surfaces of the film. Different surface patterns or roughness levels can be produced by varying the width of the discharge gap and the temperature of the die lips directly on the die exit during melt fracture extrusion.

[0027] It is preferred to perform step a) to obtain a film with a stochastic roughness of the surfaces of Rz=10 to 70 μm and more preferably a film with a stochastic roughness of the surfaces of Rz=30 to 70 μm.

[0028] In a first variant of the invention, the extrusion is performed under melt-fracture conditions with extrusion dies having a lip temperature of 100-270° C., preferably 100-240° C.

[0029] In a second variant of the invention, the extrusion under melt-fracture conditions is performed with a melt flow rate of 500-3500 kg/h.

[0030] Subsequent to extrusion, the film is subjected to embossing in step b) on one or both sides, independently in each case, with a surface structure and a roughness depth of R.sub.z=20 to 100 μm, preferably R.sub.z=20 to 80 μm, in particular R.sub.z=25 μm to 70 μm.

[0031] The surfaces of the film obtained in step a) can be embossed in a single step or preferably in two distinct embossing steps. In single step embossing, two embossing rolls are used, whereas in multiple step embossing, an embossing roller and a pressure roller is used. The pressing roller preferably has a surface of rubber with a Shore A hardness of 20-80.

[0032] Measuring the surface roughness of the film with the roughness value Rz is effected according to DIN EN ISO 4287 and DIN ISO 4288. The measuring devices used to measure the surface roughness must satisfy EN ISO 3274. The profile filters used must correspond to DIN EN ISO 11562.

[0033] The embossing step b) according to the invention can be carried out in such a way that the two sides of the structured film have different roughness depths R.sub.z. This can be achieved e.g. by different embossing tools or temperatures of the embossing tools and/or the pressing rollers.

[0034] The channels on both surfaces of the film may share an angle of 70 to 90° or 5-45° with each other. In another aspect, the channels on at least one surface of the film have an angle of 5-45°, preferably 35-45° to the direction of extrusion.

[0035] The pitch of the channels can be the same or different on the surfaces of the film, where a deviation of 5% between the surfaces is regarded as being the same. The pitch of the channels can be 100-1500 μm, preferable 300-1000 μm.

[0036] FIG. 1 shows by way of example the surface of film produced by the method of the invention with a pitch a) of 500 μm, a channel width b) of 75 μm and a surface roughness of the elevations between the channels c) of 40 μm.

[0037] Before and/or after the embossing process, the film can be cooled to −10 to +40° C. to fix the surface structure of the film in this way. Cooling preferably takes place via correspondingly temperature-adjusted cooling rollers.

[0038] Preferably, the embossing rollers are made of metal or ceramics and possess a surface with a negative profile pattern of the structure present later on in the film surface. Higher depth of channel of embossing rollers than the intended roughness of the film is preferable to keep melt fracture surface after embossing.

[0039] The temperature of the embossing rollers is preferably 80 to 200° C., especially 80 to 170° C., more preferably 100 to 160° C., and in particular 110 to 155° C. Most preferably, the embossing rollers have a coated steel surface (e.g. coated with polymer or ceramics) in order to reduce the adhesion of the film.

[0040] In a first embodiment, the extruded film is embossed between two embossing rollers having the same or different surface embossment.

[0041] In another embodiment of the invention, the film is guided between the embossing roller and the pressing roller rotating in the opposite sense. Preferably, the film is exposed, between the embossing rollers and/or embossing and pressing rollers to a line pressure of 10 to 400 N/mm, more preferably 10 to 150 N/mm, yet more preferably 30 to 130 N/mm and in particular 40 to 110 N/mm. The line pressure can be the same or different if several process steps b) are conducted. Line pressure means the pressing force of the roller pair based on the film width.

[0042] The pressing rollers preferably have a temperature of 0 to 50° C., more preferably 5 to 30° C., i.e. they are actively cooled vis-à-vis the embossing roller. The temperature of the pressing rollers may be the same or different in process steps b).

[0043] The pressing rollers press the film into the structured surface of the embossing rollers and nestle lightly against the embossing roller. By changing the line pressure, the surface of the embossing zone and consequently the residence time of the film in the roller gap can be altered.

[0044] By selecting the process parameters of line pressure, film temperature and/or roller temperature, roller speed and enveloping angle of the film web on the rollers, the roughness depth of the film embossing can be influenced with a given roughness depth of the embossing rollers.

[0045] In this case, too, the film can be guided through the roller gap of the temperature-adjustment rollers directly, i.e. without passing around them.

[0046] It is possible to use in particular polyvinyl butyral (PVB), in the crosslinked or non-crosslinked form, as a partially acetalated polyvinyl alcohol, in admixture with at least one plasticiser, and optionally dyes, pigments, metal salts for adhesion regulation, organic additives and/or inorganic fillers.

[0047] All plasticisers known in the art for this purpose, in particular the esters of multivalent acids, polyhydric alcohols or oligoether glycols, such as e.g. adipic acid esters, sebacic acid esters or phthalic acid esters, in particular di-n-hexyl adipate, dibutyl sebacate, dioctyl phthalate, esters of diglycol, triglycol or tetraglycol with linear or branched aliphatic carboxylic acids and mixtures of these esters are suitable, on the one hand, as plasticisers for the partially acetalated polyvinyl alcohols. Esters of aliphatic diols with long chain aliphatic carboxylic acids, in particular esters of triethylene glycol with aliphatic carboxylic acids containing 6 to 10 C atoms, such as 2-ethyl butyric acid or n-heptanoic acid are preferably used as standard plasticisers for partially acetalated polyvinyl alcohols, in particular polyvinyl butyral. One or several plasticisers from the group consisting of di-n-hexyl adipate (DHA), dibutyl sebacate (DBS), dioctyl phthalate (DOP), esters of diglycol, triglycol or tetraglycol with linear or branched aliphatic carboxylic acids, in particular triethylene glycol-bis-2-ethyl butyrate (3GH), triethylene glycol-bis-n-heptanoate (3G7), triethylene glycol-bis-2-ethyl hexanoate (3G8), tetraethylene glycol-bis-n-heptanoate (4G7) are used.

[0048] In a particular embodiment of the present invention, the adhesion of the film to the embossing tools can be further reduced by adding a substance reducing adhesion to the film material.

[0049] The plasticised partially acetalated polyvinyl alcohol resin preferably contains 25 to 45 parts by weight and pyrticularly preferably 30 to 40 parts by weight of plasticiser, based on 100 parts by weight of resin.

[0050] The partially acetalated polyvinyl alcohols are produced in the known way by acetalation of hydrolysed polyvinyl esters. Formaldehyde, acetaldehyde, propionaldehyde, butyraldehyde and such like, preferably butyraldehyde, for example, are used as aldehydes.

[0051] The preferred polyvinyl butyral resin contains 10 to 25% by weight, more preferably 17 to 23% by weight and most preferably 19 to 21% by weight of vinyl alcohol radicals, and/or 0 to 20% by weight, preferably 0.5 to 2.5% by weight of acetate radicals.

[0052] In a further process variation, a PVB partially crosslinked with a polyaldehyde (in particular glutaraldehyde) and an oxocarboxylic acid (in particular glyoxylic acid) is used as polymer according to WO 2004/063231 A1. Such a partially crosslinked PVB has a viscosity which is 10 to 50% higher than that of the analogous non-crosslinked PVB.

[0053] The water content of the films is preferably adjusted to 0.15 to 0.8% by weight, in particular to 0.3 to 0.5% by weight.

[0054] The films produced according to the invention can be used in particular for the manufacture of laminates from one or several glass panes and/or one or several polymer panes and at least one structured film.

[0055] During the manufacture of these laminates, a pre-composite is first produced from the glass/polymer panes and the film by pressing, vacuum bag or vacuum ring. As a rule, pre-composite laminates are slightly turbid as a result of air inclusions. The final manufacture of the laminate takes place in the autoclave e.g. according to WO 03/033583.

[0056] 0.76 mm thick PVB film containing a nominal level of 38 parts plasticizer per 100 parts PVB resin is extruded by the following conditions.

[0057] Lip temperature; 190° C. [0058] Melt flow rate; 1000 kg/h. [0059] Line speed; 15 m/min

[0060] This PVB film has a melt fracture surface roughness on each side characterized by value of Rz melt fracture of 40 microns.

[0061] This PVB film is embossed in a facility with the following properties. The pressing and embossing rollers of the two embossing stages had identical properties.

[0062] Facility parameters:

[0063] Hardness of the rubber roller: 70±5 Shore A

[0064] Roughness of the embossing roller: approximately 200 m

[0065] Pitch of embossing roller: approximately 500 m

[0066] Angle of the channel: 12°

[0067] Surface coating: Polymer

[0068] Temperature of rubber roller 10° C.

TABLE-US-00001 TABLE 1 No. Line pressure (N/mm) T of embossing roller (° C.) 1 90 125 2 130 125 3 90 130 4 110 130 5 130 130 6 90 135 7 110 135 8 110 200 9 110 60

[0069] The properties of the film are shown in the following tables, wherein “Rz final” stands for the roughness after embossing, “Rz elevation” stand for the roughness of the elevation between the channels and “Channel depth” is defined as “Rz final−Rz elevation”

TABLE-US-00002 TABLE 2 upper side (m) Lower side (m) Rz Rz Channel Channel Rz eleva- Channel Channel Rz eleva- width depth final tion width depth final tion 1 75 6 46 40 75 6 45 39 2 75 9 48 39 75 10 48 38 3 75 13 51 38 75 12 50 38 4 75 14 52 38 75 14 52 38 5 75 16 54 38 75 16 54 38 6 75 21 58 37 75 20 57 37 7 75 22 59 37 75 22 59 37

[0070] During the manufacture of the composite glass, the films exhibited good air removal properties and could be processed to blister-free laminates.

Comparative Example

[0071]

TABLE-US-00003 TABLE 3 upper side (m) Lower side (m) Rz Rz Channel Channel Rz eleva- Channel Channel Rz eleva- No. width depth final tion width depth final tion 8 75 6 133 7 75 133 140 7 9 — 0 40 40 — 0 40 40

[0072] During the manufacture of the composite glass, the films exhibited bad air removal properties and could not be processed to blister-free laminates.

[0073] Especially the sample of No. 8 showed high tackiness. It was very difficult to handle this film due to high adhesion/blocking between two layers.

[0074] With the process of the invention, plasticized polyvinyl acetal film can be produced which has a low tendency of blocking. Such film can be wound to a roll for transportation and easily unrolled for production of laminated glazing.