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AU779525B2 - Method and film for producing laminated safety glass panes - Google Patents
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AU779525B2 - Method and film for producing laminated safety glass panes - Google Patents

Method and film for producing laminated safety glass panes Download PDF

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Publication number
AU779525B2
AU779525B2 AU23448/01A AU2344801A AU779525B2 AU 779525 B2 AU779525 B2 AU 779525B2 AU 23448/01 A AU23448/01 A AU 23448/01A AU 2344801 A AU2344801 A AU 2344801A AU 779525 B2 AU779525 B2 AU 779525B2
Authority
AU
Australia
Prior art keywords
film
plasticized
glass
roughness
laminated safety
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
AU23448/01A
Other versions
AU2344801A (en
Inventor
Gunter Becker
Bernhard Koll
Holger Stenzel
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Kuraray Europe GmbH
Original Assignee
Huels Troisdorf AG
HT Troplast AG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Huels Troisdorf AG, HT Troplast AG filed Critical Huels Troisdorf AG
Publication of AU2344801A publication Critical patent/AU2344801A/en
Application granted granted Critical
Publication of AU779525B2 publication Critical patent/AU779525B2/en
Assigned to KURARAY SPECIALITIES EUROPE GMBH reassignment KURARAY SPECIALITIES EUROPE GMBH Alteration of Name(s) in Register under S187 Assignors: HT TROPLAST AG
Assigned to KURARAY EUROPE GMBH reassignment KURARAY EUROPE GMBH Alteration of Name(s) in Register under S187 Assignors: KURARAY SPECIALITIES EUROPE GMBH
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
    • B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
    • B32B17/10807—Making laminated safety glass or glazing; Apparatus therefor
    • B32B17/10816—Making laminated safety glass or glazing; Apparatus therefor by pressing
    • B32B17/10825—Isostatic pressing, i.e. using non rigid pressure-exerting members against rigid parts
    • B32B17/10834—Isostatic pressing, i.e. using non rigid pressure-exerting members against rigid parts using a fluid
    • B32B17/10844—Isostatic pressing, i.e. using non rigid pressure-exerting members against rigid parts using a fluid using a membrane between the layered product and the fluid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
    • B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
    • B32B17/10009—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the number, the constitution or treatment of glass sheets
    • B32B17/10036—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the number, the constitution or treatment of glass sheets comprising two outer glass sheets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
    • B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
    • B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
    • B32B17/10559—Shape of the cross-section
    • B32B17/10577—Surface roughness
    • B32B17/10596—Surface roughness created by melt fracture
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
    • B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
    • B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
    • B32B17/10761—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer containing vinyl acetal

Landscapes

  • Joining Of Glass To Other Materials (AREA)
  • Laminated Bodies (AREA)
  • Manufacture Of Macromolecular Shaped Articles (AREA)
  • Moulding By Coating Moulds (AREA)

Abstract

The invention relates to a one-step method for producing laminated safety glass panes. Said laminated safety glass panes consists of at least two glass panes and a plasticized, partially acetalized polyvinyl alcohol interlayer. According to the non-autoclave method, a plasticized, partially acetalized polyvinyl alcohol film with a roughness Rz between 70 mu m and 150 mu m is used.

Description

WO 01/30568 1 PCT/DE00/03708 Process and film for producing laminated safety glass Background of the invention The invention relates to a process and a film for producing laminated safety glass, composed of at least two panes of glass and of an intermediate layer made from plasticized, partially acetalized polyvinyl alcohol, in particular of plasticized polyvinyl butyral (PVB), in a single-stage process not using an autoclave.
Laminated safety glass, composed of two panes of glass and of an adhesive film which bonds the panes of glass and is made of polyvinyl butyral (PVB) for example, are used in particular as windshields in motor vehicles, and one pane of glass here may if desired be replaced by a sheet of plastic, especially one made from an amorphous polyamide, or from a transparent PMMA, polycarbonate or polyester. The construction sector, too, uses this type of silicate glass/silicate glass laminate or silicate glass/plastic laminate as window glass or as partitioning, for example. Here, if desired and depending on the application, e.g. bulletproof glass, use may also be made of multiple laminates, i.e.
laminates which are composed of more than two loadbearing layers.
Whereas laminated safety glass for the construction sector is intended to have, inter alia, the highest possible adhesion between glass and adhesive film, in laminated safety glass for motor vehicles it is desirable to have a specified adhesion level which is not too high.
Wherever the term polyvinyl butyral (PVB) is used in this application, it is intended to include other polymers whose properties affecting their usability are similar to those of (plasticized) polyvinyl butyral.
These include partially acetalized polyvinyl alcohols in general, and, for example, unplasticized ethylene- 2 vinyl acetate copolymers. Particular properties :egarded as relevant here are surface tack, sQftness And elastomeric properties at room temperature.
Description of the prior art Plasticized films based on polyvinyl butyral (PVB) used for producing laminated safety glass are very soft and tacky, even at room temperature. Although the high tack is indispensable for holding the glass-film-glass laminate together in laminated glass, it nevertheless has to be eliminated temporarily during transport and during processing to produce this glass. It is well known that for this purpose the films can be provided with a roughened surface on one or both sides. The roughnesses, measured as Rz to DIN 4768, are usually from 15 to 35 gm. A typical process for producing films of this type with a roughened surface is disclosed in EP 0 185 863 B1.
In producing laminate safety glass a two-stage manufacturing process is generally used. A first step prepares what is known as a prelaminate, composed of two panes of glass and of the adhesive film arranged therebetween and usually made from PVB. A second step compresses this prelaminate in an autoclave at temperatures of from about 130 to 1450C and at pressures of at least 11 bar to give the actual laminated safety glass. An example of a description of this process is given in the introduction to EP 0 331 648 A2. The water content of the PVB film used has a decisive effect on the bonding power of the laminate. It is usual to maintain a water content of from 0.40 to 0.55% by weight of the film with very tight tolerances. The use of an autoclave means that this known two-stage process is relatively complicated and requires high capital expenditure, and is therefore uneconomic for small production quantities.
EP 0 331 648 A2 discloses a process for producing laminated safety glass without using an autoclave. In 3 this known process the panes of glass, with the PVB film lying therebetween, are bonded together in an airtight evacuated sack at an elevated temperature, using the pressure of the surrounding air. That publication also discloses that, to prevent bubble formation within the laminate, the PVB film used should have the lowest possible water content. However,the drying of a film and the handling of a film dried in this way is relatively complicated.
DE 196 43 404 Al discloses another process for producing laminated safety glass without using an autoclave, by using a plasticized, partially acetalized polyvinyl alcohol film with water content below 0.35% by weight, based on the weight of the film, and with a useful content of an organosilicon-functional silane which increases adhesion. However, precise adjustment to such a low water content is very difficult.
In US 5,536,347 Al, a process for producing laminated safety glass without using an autoclave uses a PVB film which has a specific geometric structure on both sides.
Structures of this type can only be produced by using specific embossing processes and are unsuitable for many PVB-film-production plants. Other processes for producing films with regularly shaped, geometrically arranged surface structures are disclosed in DE 32 08 820 C2 and US 5,478,412 Al, but there is no disclosure here of use in a process which does not use an autoclave.
US 5,425,977 Al discloses a process for producing PVB films with a regular surface structure and with roughness Rz below 75 gm, preferably below 50 gm. There is no disclosure of use in a process which does not use an autoclave. The same applies to the process of US 4,925,725. The film described there can again only be produced by a complicated embossing process.
4 Object It is an object of the present invention to eliminate the disadvantages described while providing a process for producing laminated safety glass composed of at least two panes of glass and of an intermediate layer made from plasticized, partially acetalized polyvinyl alcohol in a single-stage process not using an autoclave which gives bubble-free laminated safety glass at a sufficient level of process reliability. A further object of the invention is to provide an intermediate layer which is made from plasticized, partially acetalized polyvinyl alcohol, can be produced without a complicated embossing process, and can be used in a process not using an autoclave.
Summary of the invention The invention achieves this object by using a PVB film with, applied to one side or preferably to both sides, a surface structure with roughness Rz 70 Mm and Rz 150 gm, preferably in conjunction with one or more features from the subclaims. If the surface roughness Rz is below 70 gm, the edges of the laminated safety glass seal during the heating phase before all of the air can be evacuated from the PVB/glass interface. This results in air inclusions (bubbles) in the center of the laminated safety glass. If the surface roughness is too high (Rz 150 gm) more energy is needed to melt the roughness peaks and the process becomes unacceptably protracted.
It is preferable for the surface structure to be applied in the extrusion process, immediately prior to discharge of the plastic melt from the extrusion die, via what may be called the flow- or melt-fracture process of EP 0 185 863 BI. Various levels of roughness can be produced as required by varying the discharge gap width and the temperature of the die lips directly at the discharge from the die. This process gives random roughness, which is approximately isotropic.
This means that the roughness value is approximately 5 the same when measured in any direction, while the individual protrusions and depressions have a random arrangement of height and distribution.
Wherever this text uses the term surface roughness Rz or roughness Rz, the surface roughness measurement is made in accordance with DIN 4768 or DIN EN ISO 4287 and DIN ISO 4288. The measurement devices used to measure surface roughness must comply with EN ISO 3274. The profile filters used must correspond to DIN EN ISO 11562.
The laminated safety glass production process preferably employed for the invention, using the film employed according to the invention, is a single-stage vacuum process based on the vacuum-ring or vacuum-sack process. In the vacuum-sack process the unbonded glass/film/glass sandwich is placed in a plastic or rubber sack. This is then sealed so as to be airtight and provided with a suction valve, preferably in the center of the pane. In the case of large-format panes it is also possible to provide two suction valves.
Using a vacuum pump, the pressure is then reduced to below 200 mbar, and evacuation proceeds for 5 min at room temperature. While retaining the reduced pressure, the sandwich is then heated to 140 0 C in a circulatingair cabinet. Depending on the heating power used, the heating rate here is from 4 to 6 0 C/min, and therefore the holding temperature of 140 0 C is reached after from 20 to 30 min. The temperature is then held at 1400C for min. Cooling must then take place to at least 600C before the pressure is restored to atmospheric pressure. Fig. 1 shows the temperature profile for this preferred one-stage process.
6 Examples of the working of the. invention, and comparative examples Example 1 Preliminary experiments are first carried out using PVB films having various roughnesses. Table 1 shows the average surface roughnesses Rz of the individual films: Film Average surface roughness R z (kpm) side 1/side 2 PVB 1 35/35 PVB 2 55/55 PVB 3 85/85 PVB 4 115/115 Table 1 Flat laminated safety glass specimens in 500 x 1100 mm format were produced by the single-stage vacuum process described above. Films PVB 1 and PVB 2 here exhibited air inclusions in the central region of the panes. This indicates that edge sealing occurred prior to complete evacuation of the panes. In contrast, films PVB 3 and PVB 4 were completely transparent. Table 2 shows a comparison of bonding properties with a laminated safety glass (PVB 4) produced by the two-stage process: Film PVB 4 Laminated safety glass Autoclave Vacuum test (two-stage process process, (single-stage comparative process, example) inventive) Moisture 0.43 0.43 Pummel adhesion F/F 5 Sn/Sn 4 4 Shear-test adhesion F/Sn [N/mm 2 13.9 13.6 Bake test in heating 140 150 cabinet at temp. Co internal bubbles 4 none Table 2 (F fire side of glass, Sn tin side of glass) 7 The values for adhesion between film and glass, expressed in Table 2 via the pummel value and the shear test, are at the same level for both types of laminated safety glass. After the test known as the bake test, which gives information on the quality of bond produced and in particular on any tendency to form bubbles, the laminated safety glass produced by the single-stage process gives no bubbles even at 150 0
C.
Example 2 (inventive) On the basis of these preliminary experiments with flat panes, two different types of windshield glass were now produced by the single-stage process. Film PVB 4 was used. Table 3 shows the dimensions of the windshields (WSS) used: Type Width Height Longitudinal Transverse flex flex min/max (mm) min/max (mm) min/max (mm) max (mm) WSS 1 1100/1410 620/660 90/30 0 WSS 2 1170/1510 660/780 110/50 17 Table 3 After the process, both windshields had satisfactory optical properties. The adhesion values and the result of the bake test correspond to the values from Example i, Table 2.
All of the films in Examples 1 and 2 were produced by what may be called the flow- or melt-fracture process of EP 0 185 863 Bl. This process gives rough surfaces with random distribution of protrusions and depressions, without any regular patterns or structures.

Claims (4)

1. A process for producing laminated safety glass, composed of at least two panes of glass andi of an intermediate layer made from plasticized, paitially acetalized polyvinyl alcohol, in. a singll-stage process not using an autoclave, which co prises using a plasticized, -partially acetalized polyvinyl alcohol film with roughness R z of from '0 to 150 Am.
2. The process as claimed in claim 1, wherein 4se is made of a plasticized, partially acethlized polyvinyl alcohol film with roughness Rz of from to 120 mm..
3. The process as claimed in claim 1 or 2, wherein use is made of a plasticized, partially acetalized polyvinyl alcohol film with random roughness structure.
4. A plasticized, partially acetalized poly vinyl alcohol film for a process as claimed in any of claims 1 to 3, where the film has roughness *z of from 70 to 150 gm. A plasticized, partially acetalized polyyinyl alcohol film for a process as claimed in claimj2 or 3, wherein the film has random roughness with z of from 80 to 150 gm. Dated this 7th day of December 2004 HT TROPLAST AG By their Patent Attorneys GRIFFITH HACK Fellows Institute of Patent and Trade Mark Attorneys of Australia COMS ID No: SBMI-01028660 Received by IP Australia: Time 16:22 Date 2004-12-07
AU23448/01A 1999-10-25 2000-10-21 Method and film for producing laminated safety glass panes Ceased AU779525B2 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19951444 1999-10-25
DE19951444A DE19951444A1 (en) 1999-10-25 1999-10-25 Automobile windscreen and wind protection plate safety glass assembly comprises plastics layer containing plasticizer sandwiched between two safety glass plates devoid of bubbles and blisters
PCT/DE2000/003708 WO2001030568A1 (en) 1999-10-25 2000-10-21 Method and film for producing laminated safety glass panes

Publications (2)

Publication Number Publication Date
AU2344801A AU2344801A (en) 2001-05-08
AU779525B2 true AU779525B2 (en) 2005-01-27

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AU23448/01A Ceased AU779525B2 (en) 1999-10-25 2000-10-21 Method and film for producing laminated safety glass panes

Country Status (13)

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EP (1) EP1235683B1 (en)
JP (1) JP4778177B2 (en)
AT (1) ATE247558T1 (en)
AU (1) AU779525B2 (en)
BR (1) BR0014983B1 (en)
CA (1) CA2388107C (en)
DE (3) DE19951444A1 (en)
ES (1) ES2204738T3 (en)
MX (1) MXPA02003874A (en)
RU (1) RU2264360C2 (en)
TW (1) TWI221830B (en)
WO (1) WO2001030568A1 (en)
ZA (1) ZA200202940B (en)

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