UA77480C2 - Process (variants) for manufacture of laminates, glass laminates produced by this process, and device (variants) for implementation of this process - Google Patents

Abstract

Glass laminates are prepared using low-water content plastic interlayer material, such as polyvinylbutyral interlayer sheets, by a process employing nip roll de-airing, and high temperature finishing at atmospheric pressure.

Description

Description of the invention

The term "unbreakable glass" usually refers to a transparent multilayer material consisting of 2 sheets of polyvinyl butyral (hereafter referred to as "sheet of PVC") sandwiched between two sheets of glass in the form of a multilayer structure. Shatter-free glass is often used to create a transparent barrier in openings in architectural structures and in car windows. Its main function is to absorb energy, for example, resulting from an impact from an object, preventing it from penetrating through the window and therefore minimizing damage to objects or injury to people inside the fenced area. Frost-free glass can also be used to provide other beneficial effects, such as to attenuate acoustic noise, to reduce the transmission of ultraviolet (UV) and/or infrared (IR) radiation, and/or to improve the aesthetic appeal of window openings.

Shatter-free glass is usually created using a technological process in which two layers of glass and an intermediate layer of synthetic material are used. for example, RUV, collect a set prepared for compression, 19 glue into a blank of multilayer material, and carry out final processing to obtain an optically transparent multilayer material. The assembly stage includes the following operations: stacking a part of glass, laying a sheet of glass on top of it, laying the second part of glass, and then trimming the excess glass along the edges of the glass layers. The gluing stage is often composite and includes the following operations: displacing most of the air from the separation boundary and partially gluing the PMV to the glass. The connection of the glass with the RUV is completed by operation 20 of the final treatment, which is usually performed at high temperature and high pressure.

The three main technological parameters are temperature, pressure and time, which can be used to achieve the corresponding goal in the process of manufacturing a multilayer material. During the final processing operation of the multilayer material, the temperature is usually raised to approximately 1402C to soften the intermediate layer, this helps it take the shape of the glass substrate surface and plastically deforms in those areas where the substrate may be on an uneven surface. distance After the intermediate layer has assumed the appropriate shape, the mobile polymer chains of the intermediate layer develop adhesion to the glass. Elevated temperature also accelerates the diffusion of residual air and/or moisture accumulations from the glass/RUV interface into the polymer intermediate layer.

Pressure plays two crucial roles in the production of laminated glass. First, the pressure contributes to the plastic deformation of the PMV by 30. Second, it suppresses the formation of bubbles, which would otherwise lead to a combined pressure of water vapor and air remaining in the system. There is no doubt that the latter role is the most significant limiting factor in the manufacture of laminated glass. When the set prepared for compression is heated at atmospheric pressure to the temperature of the final treatment, which exceeds 1009C (the boiling point of water at pressure Tatm. is equal to 1002), the water and air remaining in the set prepared for m 35 compression, (that is, in a multi-layer set consisting of non-connected layers of glass and synthetic material) tend to expand, forming bubbles. To suppress the formation of bubbles, heat together with increased pressure is usually applied to the kit in the autoclave chamber to counteract the expansion forces that occur when heating the air and water remaining inside the preform prepared for compression. -in

After all, time plays the most important role in the production of multilayer material. Despite the fact that the production of multilayer material can be accelerated due to temperature and pressure, for the production of high-quality multilayer glass, a certain critical time must always pass.

Unfortunately, even careful optimization of these three controlled process parameters is often insufficient to produce high-quality laminated glass. If there is too much air left in the laminate, which was accumulated in the previous bonding step, no amount of time, no amount of temperature, and no amount of pressure will be able to produce a good laminate. Specialists in the production of laminated glass are well aware of the exact relationship between the gases remaining at the separation boundary and the subsequent formation of 5p bubbles at high temperature, and are constantly improving the bonding process to minimize the amount of gases at the separation boundary (ee). Virtually all modern methods of manufacturing laminated glass include a bonding/deaeration step, which involves either the operation of compressing the ready-to-compress kit with pressure rollers or the operation of placing the ready-to-compress kit into a closed volume of a tank or ring and drawing it in a vacuum to remove gases. In the prior art, there are a number of different deaeration methods designed to minimize the amount of remaining air, which serve as a means of improving the bubble resistance of the multilayer material during the final stage (F) of the high-temperature final treatment. Despite this, almost all of these prior art d) multilayer manufacturing processes require a final treatment in a sealed autoclave at a pressure greater than about 10 atmospheres and at a temperature greater than about 13020 to obtain a multilayer glass of acceptable quality.

One noteworthy prior art non-high pressure method is based on an improved deaeration procedure (using an embossed RUV sheet in a vacuum process) to eliminate the need for standard autoclave processing. This process is described in US Pat

Mo5,536,347, incorporated herein by reference, in which a method of removing air in a vacuum without using an autoclave is proposed, while in the manufacture of a preliminary blank of a multilayer material, a sheet of PMV with a water content in the range of 0.4 to 0.6 weight percent is used. This method based on vacuuming without an autoclave provides such good air removal from the multilayer material blanks obtained by this method that their processing can be carried out using the stage of high-temperature final processing at atmospheric pressure, which prevents the formation of bubbles at the boundaries of separation.

It appears that the desired interlayer sheet water content used throughout the history of laminated glass has remained relatively constant in the range of about 0.30 to about 0.60 weight percent. Although, as indicated above, the relationship between residual air and bubble formation was known and investigated in the prior art, the relationship between the 7/0 water content of the RUV interlayer material and subsequent bubble formation in the multilayer material was effectively was not used as a means to an end.

It was unexpectedly discovered, in accordance with this invention, that due to a new method, which preferably includes the use of an intermediate layer of RUV, having a reduced water content, in the manufacture of a set prepared for compression, a technological process for the manufacture of a multilayer material, which is not 7 /5 needs final processing in an autoclave. The invention proposes a method of manufacturing multilayer glass, which includes the following steps: positioning a synthetic material with a moisture content of less than 0.35 percent by weight, opposite at least one rigid substrate for forming a set; preheating at least one rigid substrate or synthetic material, or any combination of them, to the gluing temperature; gluing of synthetic material with at least one rigid 2o substrate by means of short-term application of pressure to form a workpiece of multilayer material; and final heating of the preform of the multilayer material to a temperature and for a time that ensure effective bonding of the synthetic material to the substrates to form the multilayer material. In addition, the invention proposes a method of manufacturing multilayer glass, which includes the following steps: placing a synthetic material with a moisture content of less than 0.35 percent by weight between two rigid substrates to form a set; preliminary heating of at least one of the substrates or synthetic material, or any combination thereof, to the gluing temperature; gluing synthetic i) material with two substrates using a short-term application of pressure to form a workpiece of multilayer material; and final heating of the multilayer material blank to a temperature and for a time that ensures effective bonding of the synthetic material to the substrates and for forming the multilayer material. The final heating can be carried out at atmospheric pressure, thus allowing the production of laminated glasses without the need for the standard pressure autoclaving step, which has traditionally been the main prerequisite for successful production of laminated glass. "IS

In accordance with the principle disclosed in this invention, it is now apparent that there is a threshold value of the combined water and air content in the interlayer and at the boundaries of the glass/interlayer interface, below which there is no need to create a pressure greater than atmospheric to prevent the formation of bubbles at final treatment temperature values higher than 1002. In particular, it was established that if the water content (moisture) of the intermediate layer with RUV is preferably lower than approximately 0.30 weight percent, and more preferably from approximately 0.01 to approximately 0 ,20 percent by weight, then the multilayer material blank (a set with air removed from it and with a sealed edge, consisting of layers of glass and synthetic material "which are only partially connected to each other) can be transformed into a finished product (fully glued and shsh c transparent), which meets the desired requirements for the quality and reliability of the multilayer material, without the use of reduced pressure to remove air from the workpiece raw material and without final "" pressure treatment in an autoclave.

Due to the use of low-water-content РМУВ as a synthetic material for the intermediate layer, in the final processing of the multilayer material, much higher temperature values can be used at -I reduced pressure in the autoclave or even at atmospheric pressure, than previously possible temperature values when using a blank of the multilayer material with the air removed with the help of pressure rollers. and Thus, the present invention provides the possibility of manufacturing multilayer materials at atmospheric or reduced pressure in an autoclave and at a temperature in the range from approximately 1159 to approximately 2302C, and preferably from approximately 1252 to approximately 22096. In addition, realizing all the temperature-dependent advantages of using high temperatures in the 62 final step, such as dissolving air in the RUV, softening the RUV to fill the space between the rigid substrates and thereby conform to the substrate, by filling the gap between the surfaces of the substrates, the development of adhesion and reduction of residual stresses in the PMV occurs in a shorter period of time. In particular, in this technological process, the time required for the production of finished multilayer materials that meet the established technical conditions can be reduced from the usual range of i) values from approximately 360 minutes and above to less than 180 minutes, preferably from approximately , 0.5 minutes to about 180 minutes, more preferably from about 2 minutes to about 60 minutes. The high heat resistance of multilayer materials according to the invention also makes them much less sensitive to temperature changes in the process of manufacturing multilayer material, due to which they ensure an increase in the yield of suitable products.

In some processing modes, some limited pressure may be used during the final processing.

However, such final processing includes a heating operation at such a temperature and for a time that is effective for connecting the synthetic material to the substrates, at pressure values lower than the standard pressure in the 65 autoclave. Preferably, during the final processing operation, in which the synthetic material is glued to the substrates, a pressure value of less than, approximately, three atmospheres is used; atmospheric pressure is more preferably used.

The device for manufacturing multilayer material according to the invention contains: a device for primary heating, which serves to preheat a layer of synthetic material to the temperature of gluing; means of applying pressure for gluing (for example, a means in the form of pressure rollers) that provides a short-term application of pressure to a multilayer assembly consisting of at least one rigid substrate and a layer of synthetic material, for gluing the layer of synthetic material to the rigid substrate in such a way that to form a workpiece of multilayer material; and a final heating device for heating the preform of the multilayer material to a temperature and for a time that/o ensure effective bonding of the synthetic material to the rigid substrate.

Next are the drawings in which similar elements are marked with the same reference positions and in which the following is depicted:

Fig. 1 is a schematic side view showing one of the variants of the implementation of the device suitable for the practical implementation of this invention. The illustrated device includes a device for preheating, 7/5 After which there is a means in the form of pressure rollers, after which there is a device for final heating.

Fig. 2 is a schematic side view of a second embodiment of the device suitable for practical implementation of this invention. The illustrated device contains a preparation device in the form of pressure rollers, after which there is a device for preheating, after which there is a device in the form of pressure rollers, and after it there is a device for final heating.

Fig. 3 is a schematic side view of the third embodiment of the device, suitable for the practical implementation of this invention. The illustrated device contains a device for preparatory heating, after which there is a preparatory device in the form of pressure rollers, after which there is a device for preheating, after which there is a device in the form of pressure rollers, and after it c 2g5 there is a device for final heating.

Fig. 4 is a schematic side view of the fourth embodiment of the device suitable for practical i) implementation of this invention. The illustrated device includes a preparation means in the form of pressure rollers, after which there is a device for preheating, after which there is a means in the form of pressure rollers, and after it there is a vertical conveyor heating device for final heating. (in zo Fig. 5 is a schematic side view of the fifth embodiment of the device, suitable for the practical implementation of this invention. The illustrated device contains a means in the form of pressure rollers, after which a device for preheating is located, after which a second means is located in the form of "E pressure rollers, after which there is an unloading rail conveyor, after which there is a loading trolley, and after it there is a device for final heating. -

According to the invention, in the process of manufacturing a multilayer material, cha leaves from a synthetic material with a low moisture content are preferably used. If necessary, sheets of synthetic material are first pretreated to obtain a low moisture content (ie, water content) prior to assembly with rigid, transparent, preferably glass, substrates to create a compression-ready prepackage. The water content of the sheet of preferably RUV in a set prepared for compression can be as high as 0.35 weight percent, but preferably should be less than about 0.30 weight percent, and more preferably in the range of about 0.01 to about 0.20 weight percent. More preferably the content. of water takes a value in the range from approximately 0.03 to approximately 0.18 percent of the weight of the PMV sheet. and?" The PMV sheet used in this invention is serially produced by Zoishia, Ips, St. Louis,

Missouri, as an intermediate layer of "ZayehF". The thickness of the sheet is preferably from about 0.25 to 4.0 mm, and more preferably from about 0.32 to 2.5 mm, although this is not a necessary condition. -I If pretreatment of PMV is necessary to ensure the desired water content, then the time and temperature of the pretreatment of the PMV sheet to ensure low humidity are not critical. The preferred time for pre-treatment of a sheet from RUV using an oven to evaporate the water contained in the sheet is approximately 30-60 minutes at a temperature from approximately 602C to approximately 702 and at a relative humidity of ХВН)Хх in the oven , which is approximately equal to 5-1095. This mode easily ensures a reduction of the water content in the leaves from the "Zayehte" type RUV to approximately 0.06-0.13 percent by weight. Microwave radiation, infrared radiation or a similar processing mode can also be used for this. Alternatively, a standard synthetic material dryer, such as that used to dry synthetic material granules prior to extrusion, may be used.

Preferably, the intermediate layer of PMV usually contains from about 10 to about 30 percent by weight of hydroxyl groups represented in the form of polyvinyl alcohol, and the rest - mainly butyral, iF) represented in the form of polyvinyl butyral. The PMV may contain acetate or other monomers as disclosed, for example, in patents О5 4,968,744 and О5 5,130,370, which are incorporated herein by reference. The sheet may contain fillers, pigments, dyes and other impurities, which, for example, is disclosed in the above-mentioned patent O5 bo 9,130,370.

The content of the plasticizer in the PMV sheet is usually approximately 20-60 parts per 100 PMV parts.

Suitable plasticizers known in the art include, for example, those disclosed in Patents 05 4,292,372, 05 5,013,780 and 05 5,137,954, each of which is incorporated herein by reference. EP 87766581, also incorporated herein by reference, discloses a preferred plasticizer which is triethylene glycol di-2-ethyl b5 hexanoate.

In order to regulate the adhesion between the intermediate layer with PMV and the sheets of ready-made multilayer glass, agents that regulate adhesion can be introduced into the composition of RUV. Traditional compositions that reduce adhesion, as well as salts based on magnesium and potassium, can be introduced into the plasticized sheet with RUV. The preferred agent for reducing adhesion and improving the long-term stability of laminated glass is magnesium di-2-ethylbutyrate, added in concentrations ranging from approximately 0.1 to approximately 2.5 grams per kilogram of unplasticized RUV.

In addition, it is preferable to add potassium acetate at a concentration of about 0.1 to about 1.5 grams per kilogram of unplasticized RUV.

The relief of the surface of the synthetic material is not a limiting factor of this invention. For the practical implementation of this invention, a commercially available synthetic material, 7/0, can be successfully used for the intermediate layer, which has a standard surface relief. In addition, a synthetic material having a rough or structured surface with regular or irregular relief can easily be used.

Such a surface relief can be created in various ways, for example, by embossing, by cracking during melting, etc. Patents OB 5,595,818 and 05 4,654,179 describe PMV with an irregular surface relief (hereinafter "arbitrary roughness"), which is preferred for use in accordance with this invention. The reliability of the 7/5 process can be further enhanced by using a sheet of PMV with a surface relief having regular rectilinear channels, as described in patents OB 5,425,977 and 05 6,093,471, which are incorporated herein by reference. Such an RUV sheet is particularly preferred in accordance with the present invention.

As a rule, sheets made of glass and a layer or layers of PMV are collected together, and the excess part of the PMV sheet that extends beyond the edge of the glass is removed by trimming (forming a kit ready for compression).

Trimming to size can be done before or after assembly, as desired, or alternatively, after the gluing step described below.

The layers of the kit prepared for compression are heated to a temperature sufficient to bond the layers to each other in the subsequent bonding step. The temperature of gluing may vary depending on the composition of the layer of PMV (or other used layer of synthetic material). For a low modulus interlayer, sufficient bonding to hold the layers together can be achieved at room temperature. For most multilayer materials containing a single sheet of PMV sandwiched between two i) sheets of glass, sufficient bonding can be obtained at a temperature in the range of from about 409 to about 1302C, preferably from about 702 to about , 1002S. As shown in Fig. 1, the glass/RUV/glass assembly 20, referred to at this stage as the assembly prepared for compression, can be heated to the bonding temperature in a preheating device 10, which contains an enclosed furnace chamber equipped with a plurality of infrared tubular heaters 11, through which the multilayer material 20 is moved with the help of a conveyor, is located on a deck of conveyor rollers 15, which are driven by the drive motor 17. Alternatively, convection heaters, microwave radiation and other equivalent forms of heat supply, or their - 3-5 Combinations. rch-

Then, the assembly consisting of glass and interlayer of PMV is briefly applied with a bonding pressure sufficient to remove excess air at the interface between the glass and the interlayer, ensuring that the layers adhere to each other, and to seal the edges, which prevents re-" air penetration. The resulting combination of glued layers is called a multilayer material blank. The preferred method of applying pressure for gluing consists in the use of a means in the form of pressure rollers, which is known to specialists in the field of production of multilayer and shatter-free glass. As shown in Fig. 1, the means 12 in the form of pressure rollers consists of a set of pressure rollers 13 located opposite each other, having elastic surfaces, for example, of rubber, which rotate in opposite directions, providing a supply of a set 20 prepared for compression , due to the gap between these rollers. The pressure on the assembly during the short-term application of pressure is preferably carried out -And for a time of less than about 15 minutes. When using the short-term pressure application by means of the pressure rollers, the pressure is preferably applied for a period of time from about 0 .02 to about 7 about 100 seconds, and more preferably from about 0.04 to about 50.0 seconds These times are similar in duration to the bonding steps performed on conventional process lines and are significantly shorter than conventional cycle of pressure treatment in an autoclave used in serial production, duration

Me 60-150 minutes. c However, the present invention is not limited to the use of means in the form of pressure rollers to create pressure for removing air and gluing. Provided that some minimum pressure is applied to the multilayer material for a short time, the means of applying pressure for bonding are not important. Air cushions, a press using flat working surfaces, continuous belts, multiple rolls arranged in series or staggered, or the like may also be used. (i) Short-term bonding pressure as used herein describes the application of pressure to an assembly prepared for compression for a period of time sufficient to remove air and adhere the interlayer to the glass without causing permanent plastic deformation of the interlayer or forcing complete dissolution air in the intermediate layer, which occurs when using an autoclave.

The minimum pressure to be applied is preferably at least about 5 psi (0.035 atmospheres). Pressure rollers are the preferred means of short-term pressure application. The track of the rollers (the area within which the pressure is applied by the roller) in the multilayer material varies depending on the design of the pressure rollers and is usually approximately 65 equal to 1 Ohm, although this size is not critical. The force applied by the rollers to the multilayer material is preferably from about 2 to about 2000 pounds per linear inch of roller length (2-2000 pounds per linear inch (RPI); 36-35720 kilograms per linear meter; 0.014- 14.071 atmospheres)), although pressure values outside this range may be used. The time during which pressure is applied in the contact zone varies depending on the speed of passage of the multilayer material through the pressure rollers, but is usually not less than 0.02 seconds, or not more than 100 seconds. For specialists in this field of technology, it is clear that the pressure applied by means of a unit with pressure rollers is insufficient to achieve the set of results obtained in a high-pressure autoclave, that is, to displace air into the volume of the PMV, eliminate the roughness of the surface of the PMV, reduce residual stresses or the creation of complete adhesion at the interface of the RUV/glass separation. 70 After applying pressure for bonding, the bonded laminate is heated (in an oven or, optionally, in an autoclave at a pressure less than that used in standard pressure autoclave processing) for a time and temperature sufficient to develop adhesion, in order for the intermediate layer of

The PMV took the form of the surfaces and the gap between the substrates, and to relax the stresses to an acceptable level and dissolve the air. This heating dynamics may be similar to, but not limited to, that used in the traditional autoclave method developed by /5. As shown in Fig. 1, the bonded set 20 can be subjected to heat treatment, for example, in the device 14 for final heating, which contains the chambers 16 and 18 of the oven, equipped with a plurality of infrared tubular heaters 11, through which the set 20 is transported along the floor from the conveyor rollers 15 , driven by the drive motor 17. Alternatively, for the final processing of multilayer materials, convection heaters, microwave radiation and other 2o equivalent forms of heat supply, or their combinations, can be used. In the general case, the temperature values in the disclosed technological process exceed the usual temperature values in the autoclave (from 12090 to 15022), which ensures the acceleration of the multilayer material manufacturing process. In accordance with the present invention, the final processing can be carried out at about atmospheric pressure by heating the packages prepared for compression to a temperature in the range of about 115°C to about 230°C for a time preferably from about 0.5 to about 180 minutes, and more preferably from about 2 to about 60 minutes. In the production of multilayer sheet materials

PMV with a water content corresponding to the lower part of the specified range of water content values (from 0.0195 to 0.290), it is preferable to use the values of the temperature of the final treatment corresponding to the upper part of the specified temperature range; when using a sheet with a water content of less than about 0.20905, (a) especially preferred are values of the final processing temperature from about 1502 to about 22026.

On the contrary, in the manufacture of multilayer materials from a sheet of PMV with a water content corresponding to the upper part of the range of water content values (from 0.2095 to, approximately, 0.3595), it is preferable to use the "temperature" value from the lower part of the specified temperature range (from 12523 to, approximately, 15022). For example, when using a sheet with a water content within 0.2895, the values of the temperature of the final treatment are preferable,

Which is approximately equal to 1302С. After heat treatment, the finished multilayer materials are taken out of the furnace and in subject to cooling. In the practical implementation of this technological process, the prevailing pressure is atmospheric (without the use of an autoclave). Despite the fact that, according to this invention, there is no need for standard pressure treatment in an autoclave, to improve the final treatment of multilayer materials without the formation of bubbles, a limited pressure, which is preferably less than about 3 atmospheres, can be used. Also in the conditions of the invention is the implementation of the final processing stage using a set of "" heating cycles. For example, a double cycle is characterized by the fact that: primary holding for heat treatment is carried out, cooling to a temperature close to room temperature is carried out, second holding for heat treatment at a temperature , which may or may not be equal to the temperature of the initial exposure, and carry out final cooling to room temperature. Such a stage of final processing is often this. is useful for accelerating or enabling the production of a multilayer material using a PMV sheet with a water content corresponding to the upper part of the specified range of values, at temperature values corresponding to the upper part of the specified temperature range. The values of the temperature of the final treatment in each heating cycle can take values in the range from 115 °C to 23096 o 20 for 0.5 to 180 minutes. The heating stages can be performed directly one after the other or can be separated by large time intervals, so that the duration of the intermediate cooling and/or holding stage can be from 0 minutes to 50,000 minutes. The temperatures of the intermediate cooling stage can take values in the range from -202С to 1002С. For example, a billet of multilayer material with an intermediate layer of PMV containing 0.1895 water can be subjected to final processing by placing it in a furnace, 99 programmed to heat to 1802 for 30 minutes, cool to 30 °C for 60 minutes,

HF) reheating to 18092 for 30 minutes and final cooling to room temperature

Ge within 30 minutes.

Also within the scope of the invention is the implementation of the stages of gluing and final processing at different points in time. For example, a series of preforms of multilayer material can be manufactured in the form of batches of products using the gluing step proposed in the technological process invention, which are then cooled to room temperature. The final heat treatment described herein can be performed later at a time suitable for the multilayer material fabrication device (eg, several hours later, the next day, or any later time point). This type of intermittent operation is well suited to the batch manufacturing process, in which all of the b5 multilayer blanks are produced in advance, stacked on a cart, and heated all together in a final finishing step, which is similar to the final finishing step in an autoclave, but without using the existing autoclave pressure

The technological process proposed in this invention can also be implemented in a continuous mode on existing technological lines for the production of multilayer shatter-free glass. Traditional process lines usually consist of a primary heating zone, a device for primary air removal by compression, a reheating zone and a device for repeated compression. For example, to implement this invention in the embodiment of the invention shown in Fig. 2, these technological lines can be regrouped in the following configuration: the first means 22 in the form of pressure rollers, the device 10 for primary heating (adjusted to a gluing temperature in the range of, approximately , 40 oC to, 70 approximately, 1302C, preferably from approximately 702 to approximately 1002), a means 12 in the form of pressure rollers, and a device 14 for final heating (adjusted to a final processing temperature in the range of approximately 11593 to , approximately, 2302C, preferably around 18022). With this rearrangement, the pressure rollers 13 of the first means 22 cause an extremely weak connection between the PMV and the glass of the kit 20 without removing air or sealing the edges. This connection ensures the stability of the geometric dimensions 75 of the PMV sheet during primary heating in the device 10 for primary heating, without adversely affecting the functions of removing air and sealing the edges at the stage of re-compression or gluing. If the temperature of the glass and PMV is too low to affect such a connection, a preheating device 26, such as a short oven, may be required to preheat the components of the assembly 20 to the proper temperature, located at the front of the process line before the first means 22 in the form of pressure rollers (the configuration, as shown in Fig. 3, includes the furnace of the device 26 for preparatory heating, the first means 22 in the form of pressure rollers, the furnace of the device 10 for primary heating, the means 12 in the form of pressure rollers and the device 14 for final heating with a set of furnaces).

This invention is not limited to the production of a multilayer material with an outer layer of RUV, located "M" between two sheets of glass. Metal sheets or sheets of structural or synthetic material, for example, polycarbonate sheets, can be used in combination with PMV. Alternative variants of the structure can easily be implemented, for example, layers of PMV and polyurethane, formed in the form of a multilayer structure with a rigid substrate, which is, for example, glass or polycarbonate.

For example, a multilayer material, within the scope of this invention, sequentially contains a first sheet of glass, a layer of PMV, a layer of polyethylene terephthalate (PET), a second PMV layer, and a second sheet of glass. In some cases, multilayer materials may contain sheets of metal or polycarbonate with RUV located between them. Other combinations and other synthetic materials that may be used in the present invention are known to those of ordinary skill in the art. Other synthetic materials that may be used in accordance with the present invention include materials such as, for example, polyurethane, polyethylene terephthalate, polyvinyl chloride, ionomers, polyolefin elastomers, and other similar transparent polymeric materials. In addition, they can easily include layers of structured synthetic material or layers with special properties, for example, the ability to absorb or reflect sunlight, etc.

The disclosed process can be used to manufacture curved laminated glass, such as automotive windshields, rear and side windows, as well as flat laminated glass, 70 for example, for most architectural or security applications. The disclosed technological process can be used for the production of multilayer materials that do not contain glass, as well as structures that contain more than two sheets of glass. For example, multilayer materials can be "» made of alternating sheets of PMV sandwiched between layers of polycarbonate. Alternatively, this process can be usefully applied to the manufacture of multilayer materials having alternating layers of glass and PMV. -i Operational tests and properties -1 A) Optical quality

Multi-layered materials were examined with the naked eye for visual defects such as,

ChK" for example, bubbles or areas in which there is no tight contact between the glass and the intermediate layer of polymer. An evaluation of optical distortions (lenses) created due to deviations in the thickness of the intermediate layer throughout the multilayer material was carried out by placing the multilayer test materials under the light of a high-intensity xenon lamp 62 and looking for light and dark spots created due to the lens effect.

B) Adhesion upon impact

Impact adhesion is a measure of the adhesion of a sheet of synthetic material to glass. An impact adhesive strength test was performed to approximate impact dissipation. To measure impact adhesion, laminated glasses were prepared, brought to a temperature of -172°C, and were manually struck with a 1-pound hammer in such a way as to break the glass. All broken glass that did not adhere to the layer of RUV was removed. A visual comparison was made of the amount of glass remaining adhered to a set of standards of known impact rating scales, the higher the number of the standard, the greater the amount of glass remaining adhered to the interlayer with PMV (ie, at an impact corresponding to a value equal to zero, the glass does not remain at all, and with an impact corresponding to a value equal to 10, 10095 of the surface of the layer with RUV remains attached to the glass). Impact adhesion is a dimensionless quantity.

B) Disruption of the structure during processing in the furnace

The multilayer materials were placed in an oven at 100°C for approximately 16 hours, then removed from the oven and visually inspected for bubbles. The presence of any single bubble located within the laminate outside of a 1/4 inch wide edge area along the perimeter of the laminate was considered a structural failure. If no such bubbles were found within the laminate, the laminates were placed back into the oven and the temperature was increased by 102C to 1102. After holding for one hour at 110923, the laminates were again checked for bubbles. Any multilayers that failed the test were removed. All multilayer materials that passed the test were placed back into the furnace and the temperature was increased to 102C. The multilayers were left at this temperature for one hour. This process was continued until the structure of all multilayer materials was broken.

D) Violation of the structure during boiling

Samples of the multilayer material were immersed in boiling water for two hours and then visually inspected for bubbles that had formed. Laminates that pass this test are characterized by the absence of any bubbles within the laminate, except for a 1/2 inch wide edge area along the perimeter of the laminate.

Examples

The following examples are provided to further explain the invention. The examples are for purposes of illustration and should not be construed as limiting the scope of the present invention. All proportions and percentages are by weight, unless otherwise indicated.

Example Mo 1:

Five samples of RUV sheet with an initial moisture content of 0.43905, slightly larger than the required size of the final laminate, were cut and placed in an artificial climate chamber maintained at 10 C with variable levels relative humidity. The sheets were aged at RHs of 2595, 2595, 2295, 14.595, and 695 and designated as Moi, Mo2, Mo3, Mo4, and Mo5 samples, respectively. Also, five pairs of glasses were placed in the first chamber with a temperature of 702C and relative humidity. After one hour and 15 minutes, the RMV and glasses were removed from the furnaces, assembled into (5) five separate sets, prepared for compression, subjected to an edge trimming operation, and passed through a hard rubber press (0.5 feet per minute (0 .0025 meters per second (m/s)); 30 pounds per linear inch (RPI) (536bkg/m)). After the clamping device, the first workpiece of multilayer material (sample

Мо1) was treated in an autoclave using the dynamics of pressure and temperature changes typical for (а) industrial production of multilayer material (185rvzi (1.28MPa)) and 1432С during a cycle lasting 1 hour). Samples of Mo2 and Mo5 of multilayer material blanks were placed in a convection oven (at atmospheric pressure), preheated to 1802C, and held for heat treatment for 30 minutes. The MoZ sample of the multi-layer material was placed in a convection oven preheated to 1159C and held for heat treatment for 180 minutes. The Mo4 sample of the multilayer material was placed in a 3o convection oven preheated to 1302С and held for heat treatment for 90 minutes. -

After cooling to room temperature, the multi-layer materials were checked for optical transparency, moisture content, structural defects during furnace treatment, and structural defects during boiling (the results are shown in Table 1). Moi's sample had a water content of 0.3695 by weight, which is now common for laminated glass. It successfully passed all operations of Z 70 visual inspection and showed quite good characteristics when checking for structural violations caused by high temperature. The Mo2 sample of the multilayer material also had a water content equal to

From" 0.3696 by weight. It had small bubbles all over the surface of the multi-layer material and therefore failed all visual and high-temperature structural checks. A sample of Mo3 multilayer material made in accordance with embodiments of the present invention had a water content of 0.3095 by weight and was completely transparent with no visible defects. Sample

The SheMo4 multilayer material produced in accordance with embodiments of the present invention had a -I water content of 0.2095 by weight and was completely transparent with no visible defects. Finally, a sample Mob of the multilayer material made in accordance with the preferred embodiments of the present invention had a water content of 0.1195 by weight and was completely transparent with no visible defects. Samples of MoZ, Mo4 and Mob at 20 successfully passed both tests for the presence of structural violations caused by high temperature. Sample

Mo5 of the multilayer material had an extremely high temperature of occurrence of structural disturbances during micro-processing in the furnace, which was equal to 2302С. It is typical of multilayer materials made in accordance with preferred embodiments of the present invention (and those characterized by a water content in the range of from about 0.03 to about 0.18 weight percent relative to the weight of the PMV sheet), falling into the temperature range from 17092С to 2502С, in contrast to multilayer materials manufactured according to

HF) of the known state of the art, for which this temperature range is from 115922 to 1602. Samples Mo1, MoZ3, Mo4 and Mob

The multilayer materials successfully passed all optical tests, as they did not have any bubbles, non-glued areas or significant optical distortions when viewed under high-intensity light radiation. processing in the furnace 65 in the autoclave) successfully successful 2 Without processing in the autoclave 0.36 Failed inspection | Failed inspection Failed inspection

ANNE IS SUCCESSFULLY SUCCESSFULLY SUCCESSFULLY SUCCESSFULLY

Example of Mo2:

Four samples of PMV, labeled as samples Mo1-Mo4, were cut, having a slightly larger size than the 70 required size of the final multilayer material. My sample (the control sample) was cut from a standard sheet that is serially produced by the Zoitschia Ips company. The sheet of sample Me2 was identical to the control sample (sample Mo1), except that it contained 0.76 grams of magnesium di-2-ethylbutyrate and 0.29 grams of potassium acetate per kilogram of unplasticized polymer. Sample Mo3 was identical to the control sample (sample Mo1), except that it contained 1.016 grams of magnesium di-2-ethylbutyrate and 0.392 grams of potassium acetate per kilogram 75 of unplasticized polymer. Sample Mo4 was identical to the control sample (sample Mo1), except that it contained 1.27 grams of magnesium di-2-ethylbutyrate and 0.49 grams of potassium acetate per kilogram of unplasticized polymer.

The glass used for the production of multilayer materials in samples Mo1, Mo2, Moz and Mo4 was obtained from the company RITT5VOKON RAIMT AMO SI ABZ SOMRAMU (RRO), Pittsburgh, Pennsylvania, USA, which is known to provide adhesion of RMV to glass , comparable to other products of the glass industry.

The glass and PMV were placed in an oven, in which the temperature was maintained at 70 2С, and the relative humidity was maintained for 60 minutes. They were then pulled from the furnace, assembled into sets, prepared for compression, edge-trimmed, passed through a hard rubber press (0.5 ft per minute (0.0025 m/s), 30 psi RI! ( 536kg/m)) and heated in a convection oven at 1802C for 30 minutes. with

The finished multilayer materials were tested for adhesion strength by means of the impact test described in the "OPERATIONAL TESTS" section. The results obtained show that there are a number of ways to reduce the adhesion in the multilayer materials made in accordance with the present invention to moderate levels. The moisture content in the intermediate layer of the finished multilayer material was determined, which ranged from 0.08 to 0.1095 percent by weight of water. (av) so "

S da Rv t zv m

Example Mo 3: "

A sample of PMV sheet was cut slightly larger than the required size of the final laminate and placed without a glass backing in an oven maintained at 709C and 695 RH for 20-30 minutes or until the water content in the leaf will not be less than 0.1 percent by weight. Two sheets of glass were also placed in the furnace, where they were stabilized to a temperature of 7020. Then, the PMV and glass were removed from the furnaces, stacked at room temperature, subjected to an edge trimming operation and passed through a pressing device made of hard rubber (0.5 feet per minute (0.0025 m/s); 33 pounds per linear inch RI! (5Sbkg/m)). After passing through the pressing device, the multilayer material was placed in a convection oven (at atmospheric pressure), which was preheated to 180 9C, and held for -1 heat treatment for 10 minutes. It was then removed from the oven and left to cool. It is expected that the operational properties should be comparable to the operational properties of the Mo5 sample from the Mo1 example described above. so 50 Example Mo 4:

The RMV roll is unwound and fed into a chamber heated to 502C with a relative humidity of 695. The residence time of the sheet (ze) in the chamber is 25-35 minutes and is sufficient to reduce the water content to less than 0.10 percent by weight. After leaving the chamber, the RUV is placed between two sheets of glass and the edges are trimmed along the edges of the multilayer material. As shown in Fig. 1, the multilayer material 20 is then moved on conveyor rollers 15, where it is heated to 709 by means of infrared (14) tubular heaters 11,

GF) are passed through pinch rollers 13 (30 psi RI (536 bkg/m) rotating at 0.5 ft per minute (0.0025 m/s)) and moved through a final heat device 14 (in which where the heating of the multilayer material 20 with the help of infrared tubular heaters 11 to 1759 for 3 minutes without holding at a high temperature). After passing through a short cooling zone, the multilayer material 20 is pulled from the output end (when passing from left to right in Fig. 1) of the roller conveyor formed by the conveyor rollers 15. It is expected that the operational properties should be comparable to the operational properties of the above-described sample Mo5 from example Mo1.

Example Mo 5:

The RMV roll is unwound and fed into a chamber heated to 502C with a relative humidity of 695. The residence time of the sheet in the chamber is 25-35 minutes and is sufficient to reduce the water content to less than 0.10 percent by weight. After leaving the chamber, the PMV is placed between two sheets of bent glass, such as that used in side windows of cars, and the edges are trimmed along the edges of the multilayer material. The laminated material is then moved onto a conveyor where it is heated to 7023 by Convection heating, passed through segmented pinch rollers (which are a plurality of rotating discs approximately 1 inch thick, each providing a pressure of 30 psi ( RI I) (53bkg/m) rotating at a speed of 0.5 ft per minute (0.0025m/s)) and are moved through a zone of smooth convection heating in which the multilayer material is heated to 1602 and held at this temperature for 20 minutes After passing through a short cooling zone, the multilayer material is removed from the 70 conveyor. It is expected that the operational properties should be comparable to the operational properties of the Mo5 sample described above from the Mo1 example.

Example Mo 6:

A roll of RMV with a water content in the sheet equal to 0.1 percent by weight is unwound on a sheet of glass. A second sheet of glass is placed on top of it and the edges of the set are trimmed to remove excess RUV. 75 with reference to FIG. 5, a stack of multilayer material 20 is passed through a first assembly of pressure rollers 23 operating at 30 psi and at a speed of 10 feet per minute to create a light bond of glass to the LMW, but such , which is insufficient to seal the edges. Then the multilayer material 20 is moved through the device 10 for primary heating with infrared radiation, in which the set of multilayer material is rapidly heated to 10 es. After heating, the multilayer material 20 is passed through a second assembly of 12 pinch rollers, also adjusted to pressure of 33 pounds per linear inch (PI!) (53bkg/m) and a speed of 10 feet per minute (0.051m/s), which provides air removal from the boundary separation of glass/GRP, bonding of materials to each other and sealing of edges to prevent re-infiltration of air. The processed multi-layer material 20 comes from the assembly 12 of the pressure rollers onto the roller platform 28, and then it is placed on the cart 30. This procedure is repeated "CM

Until the cart 30 is filled with glued, but not yet finished products of multilayer material 20. o

The trolleys 30 then roll into the final heating device 32, which in this embodiment is a large oven that heats all the sets to 1802 and maintains this temperature for 20 minutes before cooling back to room temperature. It is expected that the operational properties should be comparable to the operational properties of the Mo5 sample described above from the Mo1 example. | "in)

Example Mo7: co

A roll of RMV with a water content in the sheet equal to 0.1 percent by weight is unwound on a sheet of glass. A second sheet of glass is placed on top of it and the edges of the set are trimmed to remove excess RUV. As shown in Fig. 4, the RMV of the multilayer material 20 having a structure of glass-PMP-glass is passed through m the first assembly of pressure rollers 22, which operates at a pressure of 30 pounds per linear inch (PI) (536 kg/m) and at a speed of From a foot per minute (0.015m/s), to create an easy gluing of glass with RMB, but such that it is - not enough to seal the edges. Then the multilayer material 20 is moved through the device 10 for primary heating with infrared radiation, in which the set of multilayer material is rapidly heated to 702C. After heating, the multilayer material 20 is passed through a second assembly of 12 pinch rollers, also adjusted to a pressure of 30 psi (536 bkg/m) and a speed of 3 feet per minute (0.015 m/s), which provides air removal from glass/UVB separation boundaries, gluing materials to each other and sealing the edges to prevent re-infiltration of air. After exiting the pressure roller unit 12 h, the multilayer material 20 (at the stage of the multilayer material blanks) is turned vertically using the vertical conveyor device 33 and is processed in the device 34 for final heating, which in this configuration includes an oven with a convection zone heating, heated to 2009C, followed by a short cooling zone. The total time spent in the heating and cooling zones is 30 and 10 minutes, respectively. (A continuous vertical conveyor is widely used in the -I branch of industrial production of multilayer materials and can be purchased from Tatadiazv, Sweden.)

It is expected that the operational properties of the finished multilayer materials should be comparable to the operational properties of the above-described sample Mo5 from example Mo 1. c 20 Some modifications may be made in the details of the invention described above, without going beyond the essence and scope of this invention, formulated in the attached formula. Therefore, it is understood that all information contained in the above description or shown in the accompanying drawings should be interpreted as illustrative and not restrictive in nature. at

Claims (34)

The formula of the invention where 1. A method of manufacturing a multilayer material, containing the following steps: positioning a synthetic material with a moisture content of less than 0.35 percent by weight in relation to its weight, opposite at least one rigid substrate, preheating at least one rigid substrate or synthetic material, or any combination thereof, to the bonding temperature, bonding the synthetic material to the substrate by briefly applying pressure to form the multilayer material blank and heating the multilayer material blank to a temperature and for a time that ensures effective bonding of the synthetic 65 material to the substrates, and the heating is carried out at a pressure in the range from about 1 to about 3 atmospheres. 2. The method according to claim 1, which is characterized by the fact that it contains the following steps: placing a synthetic material having a moisture content of less than 0.35 percent by weight between two rigid substrates, preheating at least one of the substrates or the synthetic material or any of them combinations to the bonding temperature, bonding the synthetic material to the substrates by briefly applying pressure to form the preform of the multilayer material and heating the preform of the multilayer material to a temperature and for a time that ensures effective bonding of the synthetic material to the substrates. C. The method according to claim 2, characterized in that the preheating is performed at a temperature in the range of 70 from about 402C to about 13020. 4. The method according to item C, which is characterized in that the preheating is performed at a temperature in the range from about 702C to about 10020. 5. The method according to claim 2, characterized in that the duration of the short-term application of pressure is less than approximately 15 minutes. 6. The method according to claim 5, characterized in that the duration of the short-term application of pressure is from about 0.02 to about 100 seconds. 7. The method according to claim 6, characterized in that the duration of the short-term application of pressure is from about 0.04 to about 50 seconds. 8. The method according to claim 2, which is characterized by the fact that the short-term application of pressure is performed at a pressure equal to at least approximately 0.035 atmospheres. 9. The method according to claim 2, characterized in that the heating is carried out to a temperature in the range of about 11592 to about 23020. 10. The method according to claim 9, which is characterized in that the heating is carried out to a temperature in the range from about 1252 to about 22026. si 11. The method according to claim 2, which is characterized by the fact that the heating is carried out during a time interval (5) from about 0.5 to about 180 minutes. 12. The method according to claim 11, which is characterized by the fact that the heating is carried out for a period of time lasting from about 2 to about 60 minutes. 13. The method according to claim 1, which is characterized by the fact that the heating is carried out at a pressure equal to approximately 1 (a) atmosphere. co 14. The method according to claim 2, which is characterized by the fact that the synthetic material is a sheet of polyvinyl butyral. 15. The method according to claim 14, which is characterized by the fact that at least one of the above substrates is glass. "AND 16. The method of claim 14, wherein the polyvinyl butyral sheet has a moisture content of less than about 0.30 percent by weight. 17. The method according to claim 16, which differs in that the moisture content is from about 0.01 to about 0.20 - weight percent. 18. The method of claim 17, wherein the moisture content is from about 0.03 to about 0.18 percent by weight. " 19. The method according to claim 2, which is characterized by the fact that a plurality of layers of synthetic material are located between two rigid substrates. - with 20. The method according to claim 2, which differs in that the short-term application of pressure is carried out with the help of pressure rollers. is" 21. The method according to claim 20, characterized in that the short-term application of pressure is carried out at a pressure of from about 0.014 to about 14.071 atmospheres. 22. The method according to claim 19, which is characterized by the fact that at least two of the plurality of layers of synthetic material consist of different types of synthetic material. -1 23. A method of manufacturing a multilayer material comprising the following steps: placing a sheet of polyvinyl butyral having a moisture content of about 0.01 to about 0.20 percent by weight between two rigid substrates, bonding the polyvinyl butyral to the substrates, and sealing the faces for 50 forming a preform of multilayer material and passing the preform of multilayer material through a means of briefly applying pressure for about 0.02 to about 100 seconds and heating to a temperature of about 1502 to about 2202C for a time period of about 0.5 to about 180 minutes to joining polyvinyl butyral with substrates and forming a multilayer material. 24. The method according to claim 23, which is characterized by the fact that the heating is carried out at a pressure equal to approximately 1 2 atmospheres. Gee! 25. The method according to claim 23, which is characterized by the fact that it includes the step of pre-processing the polyvinyl butyral sheet by reducing the moisture content to a value of from about 0.01 to about 0.20 weight percent. 26. Laminated glass made according to the method according to claim 1. 60 27. Laminated glass made according to the method according to claim 2. 28. Laminated glass made according to the method according to claim 23. 29. Laminated glass having an interlayer moisture content in the range of about 0.03 to about 0.18 weight percent and having a furnace breakdown temperature in the range of about 1709C to about 25096. b5 30. Apparatus for making multi-layer glass containing: a means of primary pressure application, made with the possibility of short-term application of pressure to the kit prepared for compression, which is a non-glued multilayer kit consisting of two sheets of glass substrate with a layer of synthetic material located between them, a primary heating device, made with the possibility of preheating the layer of synthetic material of the kit, prepared for compression, to the temperature of gluing and a means of applying pressure for gluing, made with the possibility of short-term application of pressure to the set prepared for compression, for gluing a layer of synthetic material with sheets of glass for forming the structure of a workpiece of multilayer material and a device for final heating, made with the possibility of heating workpieces of multilayer material to the temperature and during the time, which ensure /o effective connection of the synthetic material with the glass substrates. 31. The device according to item 3, containing: a preparatory heating device, made with the possibility of pre-heating a layer of synthetic material of a set prepared for compression, a means of primary compression, made with the possibility of short-term application of pressure to a set prepared for compression, which is a non-glued a multi-layer kit, which consists of two sheets of glass substrate, between which /5 is a layer of synthetic material and a device for primary heating, made with the possibility of pre-heating the layer of synthetic material of the kit prepared for compression to the gluing temperature, a unit for applying pressure for gluing, which provides a short-term application of pressure to the set prepared for compression, for gluing a layer of synthetic material with sheets of glass to form the structure of the multilayer material blank and a device for final heating, made with 2 o possibility of heating the multilayer material blank to the temperature and during the time that ensure the effective connection of the synthetic material with the glass substrates. 32. The device according to claim 30, which differs in that the means of applying pressure is a means in the form of pressure rollers. 33. The device according to claim 30, which is characterized in that the final heating device functions at a pressure in the range from about 1 to about 3 atmospheres. 34. The device according to claim 33, which is characterized by the fact that the final heating device functions at a pressure that i) is equal to approximately 1 atmosphere. "c) (ee) " in and - - and? -i -i sh" (ee) (42) ime) 60 b5