CN114158259A - Method for laminating composite sheets without autoclave - Google Patents

Method for laminating composite sheets without autoclave Download PDF

Info

Publication number
CN114158259A
CN114158259A CN202180002043.1A CN202180002043A CN114158259A CN 114158259 A CN114158259 A CN 114158259A CN 202180002043 A CN202180002043 A CN 202180002043A CN 114158259 A CN114158259 A CN 114158259A
Authority
CN
China
Prior art keywords
mbar
temperature
stacking sequence
equal
absolute pressure
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.)
Pending
Application number
CN202180002043.1A
Other languages
Chinese (zh)
Inventor
C·舒尔格斯
S·吉尔
N·博奇曼
M·科威兹
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.)
Saint Gobain Glass France SAS
Original Assignee
Saint Gobain Glass France SAS
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 Saint Gobain Glass France SAS filed Critical Saint Gobain Glass France SAS
Publication of CN114158259A publication Critical patent/CN114158259A/en
Pending legal-status Critical Current

Links

Images

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
    • B32B17/10009—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
    • B32B17/10009—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
    • B32B17/10082—Properties of the bulk of a glass sheet
    • B32B17/10119—Properties of the bulk of a glass sheet having a composition deviating from the basic composition of soda-lime glass, e.g. borosilicate
    • 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
    • B32B17/10587—Surface roughness created by embossing
    • 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
    • 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
    • B32B17/10807—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
    • B32B17/10853—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 the membrane being bag-shaped
    • 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
    • B32B17/10871—Making laminated safety glass or glazing; Apparatus therefor by pressing in combination with particular heat treatment
    • 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
    • B32B17/10972—Degassing during the lamination
    • 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
    • B32B2250/00—Layers arrangement
    • B32B2250/03—3 layers

Landscapes

  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Casting Or Compression Moulding Of Plastics Or The Like (AREA)
  • Joining Of Glass To Other Materials (AREA)

Abstract

The present invention relates to a method for laminating a composite sheet without autoclave, wherein: (a) -producing a stacking sequence (1) at least from a base sheet (2), at least one intermediate layer (3) and a cover sheet (4); (b1) placing a vacuum ring or bag around the stacking sequence (1); (b2) for the stacking sequence (1) -over a duration T greater than or equal to 5min, and-at a temperature T of 0 ℃ to 40 ℃, -evacuating by applying an absolute pressure p less than or equal to 300 mbar at the vacuum ring or bag; (b3) the stacking sequence (1) -is heated at an absolute pressure p of less than or equal to 300 mbar, -to a temperature T of 40 ℃ to 70 ℃, and-at a temperature gradient of less than 7 ℃/min; (b4) heating the stacking sequence (1) -to a temperature T of 90 ℃ to 140 ℃ and-to an absolute pressure p of 300 mbar to 950 mbar; (b5) stacking sequence (1) -at an absolute pressure p of 300 mbar to 950 mbar; -maintaining at a temperature T comprised between 90 ℃ and 140 ℃ for a duration T greater than or equal to 1 min; (c) the stacking sequence (1) is cooled to a temperature T of less than 40 ℃ and the vacuum ring or bag is vented and removed.

Description

Method for laminating composite sheets without autoclave
Technical Field
The present invention relates to a method of laminating composite sheets without an autoclave.
Background
Composite sheets have a variety of uses, for example as vehicle glazing, such as windshields, side, rear or roof glazings in water, land or air vehicles, as architectural glazing, fire protection glazing, safety glazing or in furniture and in movable or fixed fittings.
Composite sheets generally comprise two sheets, for example a base sheet and a cover sheet, which are connected to one another by one or more interlayers, for example made of thermoplastic polyvinyl butyral (PVB) film, under the action of heat and pressure in a lamination process.
The lamination processes customary in industry generally comprise a degassing process in combination with an autoclave process, as disclosed, for example, in DE 19903171a 1. The autoclave process is typically very time consuming and energy intensive.
Lamination processes which do not use autoclaves generally have the disadvantage that the sheets are only insufficiently connected to one another and do not meet the customary requirements, for example in the vehicle sector. Further, composite sheets that are not laminated using an autoclave typically show air inclusions and haziness in the edge regions of the composite sheet. Therefore, special interlayers are often used in lamination processes that do not use autoclaves.
DE 19643404 a1 discloses a process without autoclave, in which composite sheets are produced from plasticizer-containing and partially acetalized special polyvinyl alcohol films having a very low water content of less than 0.35% by weight, based on the film mass, and an effective content of adhesion-promoting silicon-organofunctional silanes. Such methods that do not use autoclaves include a one-step vacuum process in which the sheet is heated to a temperature of 130 ℃.
US 2009/0126859 a1 discloses a process without the use of autoclave, wherein a composite sheet is made by a special ionic polymer membrane.
Other lamination processes without autoclave are known from US 5536347 a and WO 2009/039053 a 1. A lamination process without autoclave with a combined calender process is known from WO 2017/102656 a 1.
Disclosure of Invention
The object of the present invention is to provide an improved method for laminating composite sheets without using autoclaves, which method allows cost-effective production of high-quality composite sheets.
According to the invention, the object of the invention is achieved by a method for laminating composite sheets without using an autoclave according to independent claim 1. Preferred embodiments follow from the dependent claims.
The method of the invention comprises at least the following method steps:
the method according to the invention comprises at least the following method steps:
the first step is as follows:
(a) a stacking sequence is produced at least from a base sheet, at least one intermediate layer and a cover sheet, which are laminated to a composite sheet by the method according to the invention.
Following one step for degassing the stacking sequence, comprising the steps of:
(b1) placing a vacuum ring or bag around the stacking sequence;
(b2) venting of the stack sequence (so-called "cold venting")
At a temperature T of from 0 ℃ to 40 ℃, preferably at a temperature of from 0 ℃ to 30 ℃, particularly preferably at a temperature of from 0 ℃ to 25 ℃ and in particular at room or ambient temperature,
over a duration t of greater than or equal to 5 minutes (abbreviation: min), preferably over a duration t of from 5min to 15min and particularly preferably over a duration t of from 7min to 12min, and
by applying an absolute pressure p of less than or equal to 300 mbar, preferably less than or equal to 200 mbar and particularly preferably less than or equal to 150 mbar to the vacuum ring or vacuum bag;
(b3) heating the stacked sequence
-a temperature T of from 40 ℃ to 70 ℃, preferably from 55 ℃ to 65 ℃,
at an absolute pressure p of less than or equal to 300 mbar, preferably less than or equal to 200 mbar and particularly preferably less than or equal to 150 mbar, and
-at a temperature gradient of less than 7 ℃/min, preferably from 3 ℃/min to 6 ℃/min;
(b4) venting a stacking sequence
By applying an absolute pressure p of 300 mbar to 950 mbar, preferably 500 mbar to 900 mbar, to the vacuum ring or bag, and
-heating the stacked sequence to a temperature of 90 ℃ to 140 ℃, preferably 100 ℃ to 130 ℃ and especially 110 ℃ to 125 ℃;
(b5) further venting of the stacking sequence
-by keeping the absolute pressure p at the vacuum bag or vacuum ring in the range of 300 mbar to 950 mbar, preferably 500 mbar to 900 mbar, and
-maintaining the temperature T of the stacking sequence in the range of 90 ℃ to 140 ℃, preferably 100 ℃ to 130 ℃ and especially 110 ℃ to 125 ℃,
-over a duration t greater than or equal to 1min, preferably from 1min to 30 min.
And a stacked sequence of cooling and ventilation, comprising at least the steps of:
(c) the stack sequence is cooled to a temperature T of less than 40 ℃ and the vacuum ring or vacuum bag is vented and removed.
The pressure indicated always relates within the scope of the invention to absolute pressure, i.e. pressure relative to an absolute vacuum of p =0 bar. Thus, a value of 0 mbar corresponds to an ideal vacuum, while a value of 1013.25 mbar corresponds to a normal pressure under standard conditions.
An absolute pressure of 300 mbar is thus a pressure which is 300 mbar higher than the pressure of an absolute (i.e. ideal) vacuum of p =0 mbar. An increase in the absolute pressure p within the scope of the invention means an increase in the absolute value, i.e. for example from 100 mbar (ideal vacuum relative to 0 mbar) to 200 mbar (ideal vacuum relative to 0 mbar). An absolute pressure of 0 mbar to 950 mbar can therefore also be referred to as negative pressure, since this is lower than normal under standard conditions.
It goes without saying that further sheets or, for example, functional sheets or functional elements can also be arranged between the base sheet and the cover sheet in the stacking sequence, wherein a composite sheet having only the cover sheet and the base sheet as the sheets is preferred.
In an advantageous embodiment of the process according to the invention, the absolute pressure p in process step (b4) is greater than 300 mbar and in particular greater than 500 mbar at a temperature T greater than or equal to 100 ℃, in order to prevent softened intermediate layers (for example PVB-films) from being sucked out of the layer stack of the stack sequence. The pressure level should always be as low as possible within the above-mentioned pressure range in order to prevent the formation of bubbles in the stacking sequence, in particular at the edges of the stacking sequence.
In a further advantageous embodiment of the method according to the invention, the stacking sequence is heated in method step (b4) with a temperature gradient of greater than or equal to 7 ℃/min, particularly preferably from 8 ℃/min to 30 ℃/min. In particular, the temperature gradient is greater than in process step (b 3). Due to the cold exhaust according to the invention, which has been completed in process step (b2), the heating can be performed speedily without compromising the quality, which saves process time.
In a further advantageous embodiment of the method according to the invention, the stacking sequence is heated to the target temperature in method step (b4) for a duration of 1min to 15 min.
In an advantageous embodiment of the method according to the invention, in method step (c), the stack sequence is first cooled to a temperature T of less than or equal to 80 ℃, preferably less than or equal to 60 ℃ and in particular less than or equal to 40 ℃, and then the vacuum ring or vacuum bag is vented and removed.
As has been shown in the course of extensive research by the inventors, the method according to the invention without the use of an autoclave leads to a particularly tight connection between the base sheet and the covering sheet, in particular in the critical edge regions of the composite sheet, and thus to particularly good sheet quality. It goes without saying that the quality of the composite sheet can be improved again by the advantageous and preferred embodiments mentioned of the method according to the invention.
Suitable as base sheet and cover sheet are essentially all electrically insulating substrates which are thermally and chemically and dimensionally stable under the conditions of manufacture and use of the composite sheet according to the invention.
The substrate sheet and/or the cover sheet preferably comprise glass, particularly preferably flat glass, very particularly preferably float glass, and in particular quartz glass, borosilicate glass, soda-lime glass or consist of these. Alternative base sheets and/or cover sheets preferably contain or consist of a clear plastic, particularly preferably a rigid clear plastic, and in particular polyethylene, polypropylene, polycarbonate, polymethyl methacrylate, polystyrene, polyamide, polyester, polyvinyl chloride and/or mixtures thereof. It goes without saying that it is also possible for one of the sheets to comprise glass and the other sheet to comprise or consist of plastic. The substrate and/or cover sheet is preferably transparent, especially for use as a windshield or rear glass of a vehicle or other applications where high light transmission is desired. In the sense of the present invention, a sheet having a transmission of more than 70% in the visible spectral range is then understood to be transparent. But for sheets that are not in the driver's view important for traffic, for example for roof glass, the transmission can also be much smaller, for example greater than 5%.
The thickness of the substrate and/or cover sheet can vary widely and thus excellently match the requirements of the individual case. Preferably, a standard thickness of 1.0mm to 25mm, preferably 1.4mm to 2.5mm, is used for vehicle glazing, and a standard thickness of 4mm to 25mm is preferably used for homes, appliances and buildings, in particular for electric heaters. The size of the sheet material may vary widely and depends on the size of the use according to the invention. The substrate and, if possible, the cover sheet have conventional areas of 200cm up to 20m, for example in the field of vehicle engineering and construction.
The composite sheet may have any three-dimensional shape. Preferably, the three-dimensional shape has no shadow zones, so that it can be coated, for example, by cathode sputtering. Preferably, the substrate is flat or slightly or strongly curved in one or more directions in space. Especially using a flat substrate. These sheets may be colorless or colored.
The substrate and/or the cover sheet are connected to each other by at least one intermediate layer. The intermediate layer is preferably transparent. The intermediate layer preferably contains at least one plastic, preferably polyvinyl butyral (PVB), Ethylene Vinyl Acetate (EVA) and/or polyethylene terephthalate (PET). However, the intermediate layer may also contain, for example, Polyurethane (PU), polypropylene (PP), polyacrylate, Polyethylene (PE), Polycarbonate (PC), polymethyl methacrylate, polyvinyl chloride, polyacetate resins, casting resins, acrylates, fluorinated ethylene-propylene, polyvinyl fluoride and/or ethylene-tetrafluoroethylene or copolymers or mixtures thereof.
The intermediate layer can be formed by one or also by a plurality of films arranged one above the other, wherein one film has a thickness of preferably 0.025mm to 1mm, usually 0.38mm or 0.76 mm. This means that the intermediate layers can each be formed from one or from a plurality of films. Preference is given here to at least three films arranged one above the other, in particular polyvinyl butyral films having alternately different plasticity or elasticity, as is known from EP 0763420 a1 or EP 0844075 a 1.
The intermediate layer may preferably be thermoplastic and bonds the cover sheet and possibly further intermediate layers to each other after lamination of the substrate.
The method of the invention is particularly suitable for processing an intermediate layer from one or more polyvinyl butyral films. The surface of the polyvinyl butyral film can be completely or partially printed on one side or on both sides and can have any desired roughness. Such printing has the advantage that the stack sequence can be evacuated more easily by means of the surface structure. Particularly preferred is the roughness RzIs a polyvinyl butyral film of 15 to 110 mu m. RzDefined herein as the average roughness depth, i.e. over a single measurement segment lrThe sum of the height of the maximum profile peak and the depth of the maximum profile valley in (a).
In one advantageous embodiment of the process according to the invention, polyvinyl butyral films having a water content of greater than or equal to 0.35% by weight (with respect to the film mass), preferably a water content of greater than or equal to 0.4% by weight and particularly preferably a water content of greater than or equal to 0.45% by weight are used as intermediate layers. The polyvinyl butyral films are in particular silane-free.
Thus, the process of the present invention is suitable for use with standard PVB films in the industry having a water content of greater than or equal to 0.4 wt% and not having a particular adhesion promoter containing a silane. Such membranes are particularly cost-effective and can be processed well in industry. In contrast to the methods according to the prior art, no special membranes compatible with the method are required in the method according to the invention. The method according to the invention is universally applicable and particularly good results can be achieved with the described membranes.
In an advantageous embodiment, the entire production of the composite web is carried out without the use of an autoclave and in particular also without a calender. Without a calender is meant a process step without a calender method. The process according to the invention is therefore particularly energy-saving and cost-effective.
In an advantageous embodiment of the method according to the invention, the absolute pressure p is continuously applied to the vacuum ring or vacuum bag during method steps (b2) to (b 5). For technical reasons, it may be necessary to remove the vacuum line for a short time, in particular if a vacuum bag is used. The vacuum ring and vacuum bag have valves that maintain the vacuum in the ring or bag when the negative pressure line is decoupled. Decoupling may be required to transport the stacking sequence, particularly from one station to the next. The pressure may be increased by leaks in the ring/bag-stack sequence system and by venting air from the stack sequence. Preferably, the absolute pressure p is also kept less than or equal to 0.8 bar, particularly preferably less than or equal to 0.7 bar, and in particular less than or equal to 0.5 bar during the decoupling phase. It has been shown that the transient decoupling and the transient pressure rise do not significantly deteriorate the results.
The heating of the stack sequence can be carried out by all technically relevant heating devices, for example by one or more electrically operated heating radiators, for example consisting of quartz rods, by other suitable radiation sources, for example microwave radiators, by convection ovens, circulating air ovens or by a stream of hot air.
Advantageously, the heating means is arranged directly on the sheet or vacuum bag. Particularly advantageous here are electrically heatable heating plates, heating coils, heating mats or the like, which are used in particular in direct contact with one of the outer surfaces of the base sheet and/or the cover sheet.
In method step (c), the stacking sequence is cooled to the desired temperature. Particularly rapid cooling can be achieved by means of at least one cooling unit, preferably by means of a blower with or without a heat exchanger. This has particular advantages: the stacking sequence can be cooled down rapidly to the required temperature in method step (c), which leads to a reduction in the process time.
A further aspect of the invention comprises the use of the method according to the invention for producing a composite sheet for a water, land or air vehicle, in particular in a motor vehicle, train, aircraft or ship, for example as a windshield, rear window, side window and/or roof window, for a building, in particular in the entry area, window area, roof area or facade area, as a mounting in furniture and appliances.
Drawings
The invention is explained in more detail below with the aid of figures and examples. The figures are schematic and not to scale. The drawings are not intended to limit the invention in any way.
In the drawings:
figure 1 shows a flow chart of an embodiment of the method according to the invention,
FIG. 2A shows a temperature profile of an exemplary embodiment of a method according to the invention, and
FIG. 2B shows a pressure trend line diagram of the exemplary embodiment in FIG. 2A, and
fig. 3 shows a simplified diagram of a stacking sequence for manufacturing composite sheets according to the invention.
Detailed Description
Fig. 1 (fig. 1) shows a flow diagram of an embodiment of a method for laminating composite sheets without an autoclave according to the present invention.
Fig. 2A (fig. 2A) shows a temperature profile of an exemplary embodiment of the method according to the invention, while fig. 2B (fig. 2B) shows a pressure profile associated with fig. 2A. For this reason, the temperature T (° c) is plotted on the time axis T in the graph of fig. 2A. The absolute pressure p (mbar) is plotted in fig. 2B on the corresponding time axis of fig. 2A. The pressure p is given as absolute pressure, so that a value of 0 mbar corresponds to the ideal vacuum and a value of 1013.25 mbar corresponds to the normal pressure under standard conditions.
Fig. 3 (fig. 3) shows a simplified illustration of a stacking sequence for manufacturing a composite sheet according to the invention.
In a first step (a) of the method according to the invention, the stacking sequence 1 is made of, for example, a base sheet 2, an intermediate layer 3 and a cover sheet 4. The composite sheet to be manufactured by lamination without using autoclave from the stacking sequence 1 is, for example, a windshield of a passenger car.
The base sheet 2 and the cover sheet 4 are in this embodiment each approximately trapezoidal and have a slight camber, as is common for modern windshields. The base sheet 2 and the cover sheet 4 are in this embodiment equally large and arranged on top of each other. The width of the base sheet 2 and the cover sheet 4 is, for example, 0.9m, and the length on the lower edge U, i.e. on the longer base of the trapezoidal sheet, is, for example, 1.5 m. The length of the edge opposite to the lower edge U is, for example, 1.2 m. It goes without saying that in the lamination of composite sheets, such as side window glass or roof glass, smaller or larger base sheets 2 and cover sheets 4, as well as triangular or rectangular with complex elevations, can be used.
The base sheet 2 is provided, for example, to face the vehicle interior space in the mounted position; and the cover sheet 4 is provided so as to be directed outward with respect to the vehicle interior space. The base sheet 2 and the cover sheet 4 are made of soda-lime glass, for example. For example, the thickness of the base sheet 2 is 1.6mm and the thickness of the cover sheet 4 is 2.1 mm. It goes without saying that the base sheet 2 and the cover sheet 4 can also be constructed, for example, with the same thickness. The interlayer 3 is a thermoplastic interlayer and consists, for example, of polyvinyl butyral (PVB). The thickness of the intermediate layer is, for example, 0.74mm to 0.86 mm.
In step (b1) of the method of the invention, a vacuum ring is placed around the outer lateral edge of the stacking sequence 1. The vacuum ring ("green snake") consists of a vacuum-stable hose having the shape of a closed loop and having a slit on its inside, into which the outer lateral edge of the stacking sequence 1 is placed. The vacuum ring completely surrounds the side edges and the gap between the base sheet 2 and the cover sheet 4 and seals them by means of vacuum techniques. The vacuum ring is connected with an optional vacuum compensation box and a vacuum pump through a negative pressure hose. The vacuum ring, the vacuum hose, if appropriate the vacuum compensation tank and the vacuum pump form a vacuum system. The volume of the vacuum compensation tank is, for example, 1m3. The delivery capacity of the vacuum pump is, for example, 300m3And a maximum absolute final pressure of 0.1 mbar is reached. For heating the stacking sequence 1, for example, a heating plate or a heating mat, for example with about 2000W/m, is connected in direct contact with the outer side surface of the base sheet and/or the outer surface of the cover sheet2The heating power of (2). The heating plate or pad is, for example, electrically heatable and controllable with respect to its heating power. Alternatively, the stacking sequence may be conveyed to the oven together with a vacuum bag or vacuum ring, e.g. airCirculated through the furnace and heated there.
In an alternative embodiment, the stack sequence 1 may also be arranged within a vacuum bag which completely surrounds the stack sequence 1 and seals it by means of vacuum techniques. The vacuum bag can also be connected to a vacuum system via a vacuum hose and, if a vacuum is applied, to the vacuum system. Advantageously, it relates to a vacuum bag with an integrated electric heating device, preferably with about 2000W/m2The heating power of (2).
For alternative heating, the stack sequence can be conveyed together with a vacuum bag or vacuum ring into an oven, for example an air circulation oven, where it is heated, for example by a hot air stream.
In a further step (b2), the stacking sequence 1 is vented by applying an absolute pressure of, for example, p =100 mbar. The illustrated pressure is based on absolute pressure, i.e. pressure relative to an absolute vacuum of p =0 bar. The degassing takes place in this method step at a temperature T of the stacking sequence 1 between 0 ℃ and 30 ℃ and at ambient Room Temperature (RT), for example at 25 ℃. This is done over a time period t of greater than or equal to 5min and, for example, 10 min.
Fig. 2A shows an exemplary diagram of the temperature profile during the method according to the invention, while fig. 2B shows the corresponding pressure profile. The horizontal axis is divided into method steps. The two axes are not to the correct scale.
Next in step (b3), the stacking sequence 1 is heated to a temperature T of 40 ℃ to 70 ℃ and for example to a temperature of about 60 ℃. The stacking sequence 1 is heated here very slowly with a temperature gradient of about 4 ℃/min. The slow temperature increase prevents premature edge sealing and ensures a specific dwell time in the temperature range in which gases, such as evaporated water and thermally active residual air, can be sucked from the layer stacks of the stack sequence 1.
The stacking sequence 1 is here held in a temperature range of 40 ℃ to 60 ℃ for a time period t of, for example, 5min, in which a favorable cold degassing takes place.
The absolute pressure at the vacuum ring or vacuum bag of p =100 mbar is continuously maintained here. It goes without saying that the underpressure at the vacuum bag or the vacuum ring can also be applied only periodically. This is the case in particular when using a vacuum bag method, in which the vacuum bag is decoupled from the vacuum system during transport between the various positions.
Subsequently in step (b4), the absolute pressure p at the vacuum bag or vacuum ring is increased to a value of 300 mbar to 950 mbar and a value of, for example, 500 mbar. While increasing the temperature T to 90 to 140 ℃ and for example 120 ℃. The temperature increase can be carried out here with a higher temperature gradient than in step (b3), for example with a temperature gradient of 20 ℃/min.
The time interval in which the layer stack is actively heated varies as a function of the heating power and the heat transfer to the inner side of the layer stack of the stack sequence 1. As the inventors' studies have concluded, the time interval of active heating of 3min to 10min is a good target value when using a heating device with very good heat transfer, such as a self-heating vacuum bag, which achieves a direct contact of the heating pad with the at least one glass surface. Greater than or equal to 2000W/m in the case of a glass thickness of 1.6mm to 2.1mm2Is advantageous.
Advantageously, the absolute pressure p is over 300 mbar and in particular over 500 mbar at a temperature T greater than or equal to 100 ℃, in order to prevent softened interlayer 3 (PVB-film) from being sucked out of the layer stack of stack sequence 1. The pressure level should always remain as low as possible within the above-mentioned pressure range in order to prevent the formation of bubbles in the stacking sequence 1 and in particular at the edges of the stacking sequence.
Next in step (b5), the stacking sequence 1 is vented at a temperature T of, for example, 120 ℃ for a period of time T greater than or equal to 1min and, for example, 10 min. The absolute pressure at the vacuum ring or bag, p =500 mbar, is continuously maintained here. As the inventors' studies have concluded, this improves product quality, in particular reduces bubble formation.
The stacking sequence 1 is then cooled in step (c) to a temperature T of less than 40 ℃ and simultaneously or subsequently the vacuum ring or vacuum bag is vented and removed.
The cooling can be accelerated by the cooling unit, for example by a flow of air from the air of the surroundings or by air cooled by means of a blower.
It is particularly advantageous if the absolute pressure p at the vacuum bag or vacuum ring is increased to ambient pressure only after cooling at a temperature of less than or equal to 60 ℃ and, for example, at a temperature of less than or equal to 40 ℃. Cooling under negative pressure (i.e. absolute pressure less than ambient pressure) is advantageous in order to reduce the possible formation of bubbles and haze in the subsequent composite sheet.
The overall duration of the heat treatment and the underpressure treatment of the method according to the invention is, for example, only about 20 to 60 min.
As the studies of the inventors have concluded, by means of the method according to the invention, composite sheets with the same or better quality can be achieved in terms of bubble formation, haze and durability compared to the case of the autoclave-lamination method according to the prior art. The method according to the invention, which does not use an autoclave, requires shorter process times, is energy-saving and can be carried out more cost-effectively overall. This is unexpected and surprising to those skilled in the art.
List of reference numerals
1 Stacking sequence
2 base sheet
3 intermediate layer
4 cover sheet
T temperature
p absolute pressure
(a) (b1), (b2), (b3), (b4), (b5), (c) method steps

Claims (15)

1. A method for laminating a composite sheet without an autoclave, wherein,
(a) -producing a stacking sequence (1) at least from a base sheet (2), at least one intermediate layer (3) and a cover sheet (4);
(b1) placing a vacuum ring or bag around the stacking sequence (1);
(b2) for the stacking sequence (1)
-over a duration t greater than or equal to 5min, and
-at a temperature T of 0 ℃ to 40 ℃,
-evacuating by applying an absolute pressure p of less than or equal to 300 mbar at the vacuum ring or the vacuum bag;
(b3) the stacking sequence (1)
-at an absolute pressure p of less than or equal to 300 mbar,
to a temperature T of from 40 ℃ to 70 ℃, and
-heating at a temperature gradient of less than 7 ℃/min;
(b4) the stacking sequence (1)
Heating to a temperature T of 90 ℃ to 140 ℃ and
-said absolute pressure p increased to 300 mbar to 950 mbar;
(b5) the stacking sequence (1)
-at an absolute pressure p of 300 mbar to 950 mbar,
at a temperature T of between 90 ℃ and 140 ℃,
-maintaining for a duration t greater than or equal to 1 min;
(c) the stacking sequence (1)
Cooling to a temperature T of less than 40 ℃ and
-venting and removing the vacuum ring or the vacuum bag.
2. The method according to claim 1, wherein an absolute pressure p of less than or equal to 200 mbar and preferably less than or equal to 150 mbar is applied in method step (b 2).
3. The process according to claim 1 or 2, wherein in process step (b2) the temperature T is from 0 ℃ to 30 ℃, particularly preferably from 0 ℃ to 25 ℃ and in particular is room or ambient temperature.
4. The process according to any one of claims 1 to 3, wherein the duration t in process step (b2) is from 5 to 15min and preferably from 7 to 12 min.
5. The method according to any one of claims 1 to 4, wherein the stacking sequence (1) is heated in method step (b3) to a temperature T of 55 ℃ to 65 ℃.
6. The process according to any one of claims 1 to 5, wherein the temperature gradient in process step (b3) is from 3 to 6 ℃/min.
7. Method according to one of claims 1 to 6, wherein in method step (b4) the stacking sequence (1) is heated to a temperature T of 100 to 130 ℃ and/or the absolute pressure p is increased to 500 to 900 mbar.
8. The process according to any one of claims 1 to 7, wherein the temperature gradient in process step (b4) is greater than or equal to 7 ℃/min, preferably from 8 ℃/min to 30 ℃/min.
9. The method according to one of claims 1 to 8, wherein the stacking sequence (1) is maintained in method step (b5) at an absolute pressure p of 500 mbar to 900 mbar and/or at a temperature T of 100 ℃ to 130 ℃.
10. The method according to one of claims 1 to 9, wherein the applied temperature T and the applied absolute pressure p are maintained in method step (b5) for a duration T of 1min to 30 min.
11. Method according to one of claims 1 to 10, wherein glass, preferably flat glass, particularly preferably float glass, in particular soda lime glass, quartz glass or borosilicate glass and/or mixtures thereof and/or at least one film of polyvinyl butyral (PVB), preferably at least three films of polyvinyl butyral with alternately different plasticity or elasticity, arranged one above the other, are used as an intermediate layer (3) for the substrate sheet (2) and/or the cover sheet (4).
12. The method of any one of claims 1 to 11, wherein 1000W/m2To 3000W/m2And preferably 1500W/m is used in case the thickness of the base sheet and/or the cover sheet is 1.4mm to 2.5mm, respectively2To 2500W/m2The heating power of (2).
13. Method according to one of claims 1 to 12, wherein at least one electrically heated or heatable heating device, preferably at least one heating plate or at least one heating coil or at least one heating mat, is used which is in direct contact with one of the outer faces of the base sheet and/or the cover sheet, and in particular a vacuum bag with an integrated electrical heating device is used.
14. The method according to any one of claims 1 to 13, wherein the stacking sequence (1) is cooled in method step (c) by cooling, preferably by forced convection and in particular by a stream of cold air.
15. The method according to any one of claims 1 to 14, wherein the entire manufacturing of the composite sheet material is performed without a calender.
CN202180002043.1A 2020-06-17 2021-06-15 Method for laminating composite sheets without autoclave Pending CN114158259A (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
EP20180468.9 2020-06-17
EP20180468 2020-06-17
PCT/EP2021/066009 WO2021254977A1 (en) 2020-06-17 2021-06-15 Method for laminating a composite pane without an autoclave

Publications (1)

Publication Number Publication Date
CN114158259A true CN114158259A (en) 2022-03-08

Family

ID=71105352

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202180002043.1A Pending CN114158259A (en) 2020-06-17 2021-06-15 Method for laminating composite sheets without autoclave

Country Status (2)

Country Link
CN (1) CN114158259A (en)
WO (1) WO2021254977A1 (en)

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5536347A (en) 1994-09-22 1996-07-16 Monsanto Company No autoclave process for forming a safety glass laminate
FR2738772B1 (en) 1995-09-15 1997-10-24 Saint Gobain Vitrage GLAZING SOUND INSULATION SHEET
DE19643404A1 (en) 1996-10-21 1998-04-23 Huels Troisdorf Process for the production of composite safety washers
ATE224300T2 (en) 1996-11-26 2002-10-15 Saint Gobain USE OF A COMPOSITE GLASS PANE FOR INSULATING VIBRATIONS CONDUCTED BY SOLID BODY IN A VEHICLE
DE19903171C2 (en) 1999-01-27 2003-03-20 Saint Gobain Sekurit D Gmbh Method and device for laminating composite panes
EP2190663A1 (en) 2007-09-17 2010-06-02 E. I. du Pont de Nemours and Company Process for the manufacture of a glass laminate
US20090126859A1 (en) 2007-11-16 2009-05-21 Cadwallader Robert J Process for producing glass laminates
JP6552730B2 (en) 2015-12-14 2019-07-31 サン−ゴバン グラス フランスＳａｉｎｔ−Ｇｏｂａｉｎ Ｇｌａｓｓ Ｆｒａｎｃｅ Method for bonding laminated glass without using an autoclave

Also Published As

Publication number Publication date
WO2021254977A1 (en) 2021-12-23

Similar Documents

Publication Publication Date Title
CA2995434C (en) Method for autoclave-free lamination of a composite pane
EP2167436B1 (en) A method of production of a bent, coated, laminated glazing, and a resultant glazing
EP1200255B1 (en) Laminated transparency
US6261398B1 (en) Process for producing a curved laminated safety glass sheet
EP0559760B1 (en) Bilayer glazing panel
EP2858822A1 (en) Process for laminating thin glass laminates
WO2013188489A1 (en) Process for laminating thin glass laminates
CN112776425A (en) Asymmetric processing method for reducing bow in laminated structures
EP4054845B1 (en) Laminate with low-e coating on thin chemically strengthened glass and method of manufacture
CN114206609A (en) Small-radius laminated glass with complex shape
CN114158259A (en) Method for laminating composite sheets without autoclave
US20210221104A1 (en) Laminates and methods with multiple interlayers and multiple substrates
CN108349220B (en) Method for laminating composite panels
CN112389048A (en) Composite glass, and manufacturing method and application thereof
US20240208187A1 (en) Method and apparatus for forming glass laminates comprising plies with offset edges
WO2019008496A1 (en) Method for bending and laminating thin glass with cover plate
CN116852818A (en) Light laminated glass for automobiles and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
WD01 Invention patent application deemed withdrawn after publication
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20220308