TWI725639B - Polymer film and uses of the same - Google Patents

Abstract

A polymer film comprising polyvinylacetal and a laminated glass manufactured using the same are provided. The polymer film has a 45-100°C dimensional variability ranging from 20 μm to 50 μm, and at least one surface of the polymer film has a surface roughness Rz ranging from 30 μm to 55 μm.

Description

Polymer film and its application

The present invention relates to a polymer film, in particular to a polymer film with specific dimensional variability and specific surface roughness, which is suitable for the preparation of laminated glass.

Laminated glass is a kind of glass material with a composite structure formed by sandwiching a polymer film between two glass sheets and tightly joining the glass sheet and the polymer film by means of thermocompression bonding. Laminated glass is widely used in the automobile industry and construction industry because of its better impact resistance and sound insulation.

Since the preparation of laminated glass involves thermal compression bonding between the glass sheet and the polymer film, how to avoid air remaining between the glass sheet and the polymer film of the laminated glass to improve the yield is actually an important issue. A known method to prevent air from remaining between the glass sheet of the laminated glass and the polymer film is to design a texture on the surface of the polymer film to facilitate exhaust during thermal compression. However, even so, the existing polymer film is still insufficient to provide sufficient exhaust performance, and the manufacturing yield of laminated glass is still poor. Although the prior art also proposes to further improve the exhaust performance by improving the fluidity of the polymer film, this method is easy to cause the defects of delamination of edge (ie, the glass edge and the polymer film are separated). .

The present invention aims to provide a polymer film, specifically, a polymer film with specific dimensional variability and specific surface roughness, which is particularly suitable for the preparation of laminated glass. The laminated glass is tested for residual bubbles in the laminated glass. Excellent and good results can be obtained in the process without edge degumming.

Therefore, one object of the present invention is to provide a polymer film comprising polyvinylacetal, wherein: The polymer film has a 45°C to 100°C dimensional variability of 20 microns to 50 microns; and At least one surface of the polymer film has a surface roughness Rz value of 30 micrometers to 55 micrometers.

In some embodiments of the present invention, the two surfaces of the polymer film independently have a surface roughness Rz value of 30 micrometers to 55 micrometers.

In some embodiments of the present invention, the polyvinyl acetal contained in the polymer film is selected from the following groups: poly(vinyl formal), poly(vinyl formal) Aldehydes), poly(vinyl butyral), poly(vinyl valeral), poly(vinyl hexanal), and combinations thereof.

In some embodiments of the present invention, the hydroxyl content of the polyvinyl acetal is 13% to 25% by weight, wherein the hydroxyl content is measured according to JIS 6728.

In some embodiments of the present invention, the weight average molecular weight (Mw) of the polyvinyl acetal contained in the polymer film is 150,000 daltons to 250,000 daltons.

In some embodiments of the present invention, in the polyvinyl acetal contained in the polymer film, the content of polyvinyl acetal with a molecular weight of less than 50,000 Daltons is 10 mol% to 20 mol%.

In some embodiments of the present invention, in the polyvinyl acetal contained in the polymer film, the content of polyvinyl acetal with a molecular weight higher than 800,000 daltons is 1 mol% to 10 mol%.

In some embodiments of the present invention, the polymer film further contains a plasticizer, and based on 100 parts by weight of polyvinyl acetal, the content of the plasticizer may be 30 to 60 parts by weight.

In some embodiments of the present invention, the polymer film has a thickness of 0.5 mm to 1.5 mm.

In some embodiments of the present invention, the polymer film is a multilayer film.

In some embodiments of the present invention, the polymer film further contains additives selected from the following groups: dyes, pigments, stabilizers, antioxidants, flame retardants, infrared absorbers, infrared blocking agents, ultraviolet absorbers, ultraviolet rays Stabilizers, lubricants, dispersants, surfactants, chelating agents, coupling agents, bonding agents, adhesion control agents, and combinations thereof.

Another object of the present invention is to provide a laminated glass comprising a first glass sheet, a second glass sheet, and the above-mentioned polymer film disposed between the first glass sheet and the second glass sheet.

In order to make the above objectives, technical features and advantages of the present invention more obvious and understandable, the following is a detailed description of some specific implementation aspects.

The following will specifically describe some specific implementation aspects of the present invention; however, without departing from the spirit of the present invention, the present invention can still be practiced in many different forms, and the protection scope of the present invention should not be limited to the specific embodiments. Implementation status.

Unless otherwise stated, "a", "the" and similar terms used in this specification and the scope of the patent application shall be understood to include both singular and plural forms.

Unless otherwise stated, the terms "first", "second" and similar terms used in this specification and the scope of the patent application are only used to distinguish the described elements or components, and have no special meaning in themselves, especially not used In the order of representatives.

Unless otherwise stated, in this specification and the scope of the patent application, the term "dimension variability" refers to the thickness change of the polymer film between specified temperatures under specific measurement conditions. For example, the dimensional variability of 45°C to 100°C refers to the thickness change of the polymer film between 45°C and 100°C. The specific measurement conditions are described in the paragraphs of the examples below.

Unless otherwise specified, in this specification and the scope of the patent application, the term "surface roughness Rz value" refers to the ten-point average roughness of the surface and is measured according to JIS B 0601 (1994).

Compared with the prior art, the effect of the present invention is to provide a polymer film with a specific dimensional variability and a specific surface roughness Rz value, and use the polymer film to provide excellent and good results in the bubble residue test. Laminated glass without edge degumming defects. The following provides a detailed description of the polymer film of the present invention and its related applications.

1. Polymer film

1.1. Composition of polymer film

The polymer film of the present invention contains polyvinyl acetal as an essential component, and may further contain other optional components, such as plasticizers or other conventional additives, if necessary. In some embodiments of the present invention, the polymer film includes polyvinyl acetal and plasticizer or is composed of polyvinyl acetal and plasticizer.

Examples of polyvinyl acetals include, but are not limited to, poly(vinyl formal), poly(vinyl acetal), poly(vinyl butyral), poly(vinyl valeral), and poly(vinyl acetal). Acetal). The aforementioned polyvinyl acetals can be used alone or in combination of multiple types. In the following examples of the present invention, poly(vinyl butyral) is used.

In this context, plasticizers refer to chemical substances that can change the plasticity of thermoplastic resins, and can also be referred to as plasticizers. Examples of plasticizers include, but are not limited to, esters of polybasic acids or polyols, such as triethylene glycol bis(2-ethylhexanoate), tetraethylene glycol bis(2-ethylhexanoate), and tetraethylene glycol bis(2-ethylhexanoate). -Ethylhexanoate), triethylene glycol bis(2-ethylbutyrate), tetraethylene glycol bis(2-ethylbutyrate), triethylene glycol diheptanoate, tetraethylenedi Alcohol diheptanoate, dihexyl adipate, dioctyl adipate, hexyl cyclohexyl adipate, diisononyl adipate, heptylnonyl adipate, dibutyl sebacate , Bis[2-(2-butoxyethoxy)ethyl adipate], polymeric adipate, dipropylene glycol dibenzoate, tripropylene glycol dibenzoate, polypropylene glycol Dibenzoate, isodecyl benzoate, 2-ethylhexyl benzoate, propylene glycol dibenzoate, diisononyl phthalate, dibutoxyethyl terephthalate, castor Sesame oil, methyl ricinoleate, soybean oil, epoxidized soybean oil, and combinations thereof.

The conventional additives can include any substance that can adapt to improve the processability of the polymer film in the manufacturing process, or impart a specific function to the polymer film. Examples of conventional additives include, but are not limited to, dyes, pigments, stabilizers, antioxidants, flame retardants, infrared absorbers, infrared blocking agents, ultraviolet absorbers, ultraviolet stabilizers, lubricants, dispersants, surfactants, chelating agents. Mixtures, coupling agents, bonding agents, and adhesion control agents. The aforementioned additives can be used alone or in combination of multiple types. For example, the polymer film may include dyes or pigments to form a colored polymer film, or include an ultraviolet absorber or an infrared absorber to form a polymer film with an anti-ultraviolet function or to form a polymer film with an anti-infrared function.

The thickness of the polymer film of the present invention can be adjusted according to actual needs under the condition of meeting the specified dimensional variability and surface roughness Rz value of 45°C to 100°C. Generally speaking, the thickness of the polymer film can be 0.5 mm to 1.5 mm, such as 0.51 mm, 0.52 mm, 0.53 mm, 0.54 mm, 0.55 mm, 0.56 mm, 0.57 mm, 0.58 mm, 0.59 mm, 0.6 mm, 0.61 mm , 0.62mm, 0.63mm, 0.64mm, 0.65mm, 0.66mm, 0.67mm, 0.68mm, 0.69mm, 0.7mm, 0.71mm, 0.72mm, 0.73mm, 0.74mm, 0.75mm, 0.76mm, 0.77mm, 0.78 Mm, 0.79 mm, 0.8 mm, 0.81 mm, 0.82 mm, 0.83 mm, 0.84 mm, 0.85 mm, 0.86 mm, 0.87 mm, 0.88 mm, 0.89 mm, 0.9 mm, 0.91 mm, 0.92 mm, 0.93 mm, 0.94 mm, 0.95mm, 0.96mm, 0.97mm, 0.98mm, 0.99mm, 1.0mm, 1.01mm, 1.02mm, 1.03mm, 1.04mm, 1.05mm, 1.06mm, 1.07mm, 1.08mm, 1.09mm, 1.1mm, 1.11mm , 1.12mm, 1.13mm, 1.14mm, 1.15mm, 1.16mm, 1.17mm, 1.18mm, 1.19mm, 1.2mm, 1.21mm, 1.22mm, 1.23mm, 1.24mm, 1.25mm, 1.26mm, 1.27mm, 1.28 Mm, 1.29 mm, 1.3 mm, 1.31 mm, 1.32 mm, 1.33 mm, 1.34 mm, 1.35 mm, 1.36 mm, 1.37 mm, 1.38 mm, 1.39 mm, 1.4 mm, 1.41 mm, 1.42 mm, 1.43 mm, 1.44 mm, 1.45 mm, 1.46 mm, 1.47 mm, 1.48 mm, or 1.49 mm, but not limited thereto.

The polymer film of the present invention can be a single layer film composed of a single layer, or a multilayer film composed of multiple layers, as long as the polymer film as a whole meets the specified 45°C to 100°C dimensional variability and surface The roughness Rz value condition is sufficient. In the case where the polymer film is a multilayer film, the materials of each layer of the polymer film may be the same or different, and each play the same or different functional layer. The functional layer is, for example, a layer that can provide one or more of the following functions : Sound insulation function, heat insulation function, reflection function, anti-reflection function, refraction function, anti-refraction function, light splitting function, or dimming function. However, the present invention is not limited to this.

1.2. Properties of polymer film

The present invention provides a laminated glass that can obtain excellent and good results in the bubble residue test and does not have edge degumming defects by controlling the dimensional variability and surface roughness properties of the polymer film. Specifically, the polymer film of the present invention has a dimensional variability of 45°C to 100°C from 20 microns to 50 microns, and at least one surface of the polymer film has a surface roughness Rz value of 30 microns to 55 microns; Preferably, the polymer film of the present invention has a surface roughness Rz value of 30 micrometers to 55 micrometers independently on the two surfaces. For example, the polymer film may have 21 micrometers, 22 micrometers, 23 micrometers, 24 micrometers, 25 micrometers, 26 micrometers, 27 micrometers, 28 micrometers, 29 micrometers, 30 micrometers, 31 micrometers, 32 micrometers, 33 micrometers, 34 micrometers, 35 micrometers. 45°C to 100 microns, 36 microns, 37 microns, 38 microns, 39 microns, 40 microns, 41 microns, 42 microns, 43 microns, 44 microns, 45 microns, 46 microns, 47 microns, 48 microns, or 49 microns °C dimension variability, and the surface of the polymer film can have 31 microns, 32 microns, 33 microns, 34 microns, 35 microns, 36 microns, 37 microns, 38 microns, 39 microns, 40 microns, 41 microns, 42 microns, The surface roughness Rz value of 43 microns, 44 microns, 45 microns, 46 microns, 47 microns, 48 microns, 49 microns, 50 microns, 51 microns, 52 microns, 53 microns, or 54 microns.

The inventor surprisingly found that the technical effect of the present invention can only be provided when the dimensional variability of the polymer film from 45°C to 100°C and the surface roughness Rz value of at least one surface meet the above specified range, namely ,Provide laminated glass without bubbles and edge degumming defects. The technical effect achieved by the present invention is beyond the expectations of those with ordinary knowledge in the technical field, especially considering that the hot pressing temperature of general laminated glass is higher than 100°C, such as 120°C, 135°C, and 150°C In the case of or higher, those with ordinary knowledge in the technical field cannot predict that the dimensional variability in the specific temperature range of 45°C to 100°C has a critical impact on the achievement of the technical effect of the present invention.

Regarding the dimensional variability of the polymer film of the present invention from 45°C to 100°C, its adjustment means include but not limited to: adjusting the viscosity of the polymer used to form the polymer film, adjusting the hydroxyl content of the polymer, and adjusting the polymerization The molecular weight and molecular weight distribution of the material, and the addition of plasticizer. For example, the properties of polyvinyl acetal can be adjusted to provide specified dimensional variability based on one or more of the following conditions: (1) The viscosity of polyvinyl acetal at room temperature and pressure can be 70 centipoise (cps) to 110 centipoise, such as 71 centipoise, 72 centipoise, 73 centipoise, 74 centipoise, 75 centipoise, 76 centipoise , 77 cps, 78 cps, 79 cps, 80 cps, 81 cps, 82 cps, 83 cps, 84 cps, 85 cps, 86 cps, 87 cps, 88 cps, 89 Cps, 90 cps, 91 cps, 92 cps, 93 cps, 94 cps, 95 cps, 96 cps, 97 cps, 98 cps, 99 cps, 100 cps, 101 cps , 102 cps, 103 cps, 104 cps, 105 cps, 106 cps, 107 cps, 108 cps, or 109 cps; (2) The hydroxyl content of polyvinyl acetal can be 13% to 25% by weight, such as 13.5% by weight, 14% by weight, 14.5% by weight, 15% by weight, 15.5% by weight, 16% by weight, 16.5% by weight, 17% by weight, 17.5% by weight, 18% by weight, 18.5% by weight, 19% by weight, 19.5% by weight, 20% by weight, 20.5% by weight, 21% by weight, 21.5% by weight, 22% by weight, 22.5% by weight, 23% by weight %, 23.5% by weight, 24% by weight, or 24.5% by weight, the hydroxyl content is measured according to JIS 6728; (3) The weight average molecular weight (Mw) of polyvinyl acetal can range from 150,000 Daltons (daltons) to 250,000 Daltons, such as 155,000 Daltons, 160,000 Daltons, 165,000 Daltons, 170,000 Daltons , 175,000 Dalton, 180,000 Dalton, 185,000 Dalton, 190,000 Dalton, 195,000 Dalton, 200,000 Dalton, 205,000 Dalton, 210,000 Dalton, 215,000 Dalton, 220,000 Dalton , 225,000 Daltons, 230,000 Daltons, 235,000 Daltons, 240,000 Daltons, or 245,000 Daltons; (4) The content of polyvinyl acetal with a molecular weight of less than 50,000 daltons in polyvinyl acetal can range from 10 mol% to 20 mol%, such as 10.5 mol%, 11 mol%, 11.5 mol% %, 12 mol%, 12.5 mol%, 13 mol%, 13.5 mol%, 14 mol%, 14.5 mol%, 15 mol%, 15.5 mol%, 16 mol%, 16.5 mol% %, 17 mol%, 17.5 mol%, 18 mol%, 18.5 mol%, 19 mol%, or 19.5 mol%; (5) In polyvinyl acetal, the content of polyvinyl acetal with a molecular weight higher than 800,000 daltons can range from 1 mol% to 10 mol%, such as 1.5 mol%, 2 mol%, 2.5 mol% Ear%, 3 mol%, 3.5 mol%, 4 mol%, 4.5%, 5 mol%, 5.5 mol%, 6 mol%, 6.5 mol%, 7 mol%, 7.5 mol% , 8 mol%, 8.5 mol%, 9 mol%, or 9.5 mol%; and (6) The amount of plasticizer in the polymer film based on 100 parts by weight of polyvinyl acetal can be 30 to 60 parts by weight, for example, 31 parts by weight, 32 parts by weight, 33 parts by weight, 34 parts by weight are added Parts, 35 parts by weight, 36 parts by weight, 37 parts by weight, 38 parts by weight, 39 parts by weight, 40 parts by weight, 41 parts by weight, 42 parts by weight, 43 parts by weight, 44 parts by weight, 45 parts by weight, 46 parts by weight, 47 parts by weight, 48 parts by weight, 49 parts by weight, 50 parts by weight, 51 parts by weight, 52 parts by weight, 53 parts by weight, 54 parts by weight, 55 parts by weight, 56 parts by weight, 57 parts by weight, 58 parts by weight, or 59 Parts by weight of plasticizer.

The surface of the polymer film of the present invention can provide the desired surface roughness Rz value through any conventional means. For example, the process conditions can be controlled during the film forming process of the polymer film, so that the surface of the polymer film has melt fracture lines and has the desired surface roughness Rz value. Take the extruded film as an example, the lip temperature can be controlled from 180°C to 200°C, the inlet pressure of the membrane head is 120 bar (bar) to 140 bar, and the linear speed is 12 meters per minute (m/min). Up to 15 meters per minute, and the extruder output is 1500 kg/hour, to provide the desired surface roughness Rz value. Alternatively, after the polymer film is formed, the surface roughness Rz value can be adjusted and provided by the mechanical pressing method; the mechanical pressing method includes but not limited to the pressed flower wheel method and the calender wheel method, and the pressed flower wheel method Better. There are no special restrictions on the pattern of mechanical pressed flowers, such as rhombus, linear, zigzag, square, tapered, circular, approximately circular, and irregular shapes. Each of the aforementioned grain patterns can exist alone, or more than one can exist at the same time. The mechanical pressing method is a method that can be easily completed by those with ordinary knowledge in the technical field to which the present invention belongs based on the disclosure of this specification and the ordinary knowledge possessed, and will not be repeated here, but will only be illustrated in the following embodiments.

1.3. Preparation of polymer film

The preparation method of the polymer film of the present invention is not particularly limited. For example, polyvinyl acetal and optional ingredients (such as plasticizer) can be mixed and kneaded to obtain a polymer composition, and then a conventional film preparation method can be used to polymerize it. The composition is formed into a film, and if necessary, mechanical embossing is performed to provide the desired surface roughness Rz value on the surface of the polymer film. Examples of the film preparation method include, but are not limited to, calendering method, casting method, extrusion tentering method, direct extrusion method, and extrusion blow molding method.

In some embodiments of the present invention, the preparation method of the polymer film is as follows: use a mixer to mix the resinous polyvinyl acetal and plasticizer at a temperature of 100°C to 150°C and 10 rpm to 50 rpm Mix and knead for 5 minutes to 30 minutes at a rotating speed to obtain a polymer composition. After the polymer composition is cooled to room temperature, place the polymer composition in a hot press at 100°C to 200°C. The temperature of C and the pressure of 2 kg to 5 kg are hot pressed for 1 minute to 10 minutes to form a film; repeat the above film forming step as necessary and adjust the composition of the polymer composition to provide films with different functions, and laminate them Each film forms a polymer film with a multi-layer structure; if necessary, the polymer film is mechanically pressed to provide the desired surface roughness Rz value.

2. Laminated glass

The polymer film of the present invention can be used to prepare laminated glass. Therefore, the present invention also provides a laminated glass, which includes a first glass sheet, a second glass sheet, and a polymer film as described above disposed between the first glass sheet and the second glass sheet.

The first glass sheet and the second glass sheet may be the same or different, and may be any glass sheet conventionally used to prepare laminated glass, such as float glass, tempered glass, wired glass, or ordinary flat glass. The invention is not limited to this. In the following embodiments, float glass is used as the first glass sheet and the second glass sheet.

The laminated glass of the present invention can be prepared by a conventional method for preparing laminated glass in the related technical field. Generally speaking, the polymer film is sandwiched between the first glass sheet and the second glass sheet to obtain a laminate, and the laminate is pre-compressed to exhaust the air between the glass sheet and the polymer film, and then The pre-compressed laminate is placed in an autoclave and placed for a period of time under high temperature and high pressure conditions to obtain laminated glass. The pre-pressing step can be performed by hot pressing or vacuuming. The vacuuming method is commonly used in the preparation of non-planar laminated glass. The following examples have been illustrated in relevant examples, and will not be repeated here. The hot pressing method is generally carried out by a hot press, mainly used for the preparation of flat laminated glass. For example, it can be carried out in the following way: Set the conveying rate of the conveyor belt of the roller press to 2 meters per minute (m/min) to 8 meters per minute and the oven temperature is set to 150°C to 200°C, the laminate is placed on the conveyor belt so that it passes through the oven and then between a pair of rollers. The distance between the rollers is set to 5.5 mm to 6.5 mm, and then let the roll-pressed laminate cool to room temperature to complete the pre-compression.

3. Example

3.1. Measurement method description

The following specific implementations are used to further illustrate the present invention, in which the measuring instruments and methods used are as follows:

[Measurement of the molecular weight distribution of polyvinyl acetal]

Use gel permeation chromatography (GPC) to measure the molecular weight distribution of polyvinyl acetal, in which polyvinyl acetal is dissolved in tetrahydrofuran (THF), and GPC analysis is performed under the following conditions , And calculate its molecular weight based on the ratio of the area of the corresponding polystyrene standard (Waters PS STD). Device: Waters 1515 PUMP system Detector: Waters 2414 RI Extraction conditions: 1.0 ml/min (mL/min), THF Column: Waters Styragel HR5 THF, Waters Styragel HR4 THF, Waters Styragel HR3 THF, Waters Styragel HR1 THF

[Measurement of the viscosity of polyvinyl acetal]

Measure the viscosity of polyvinyl acetal in accordance with JIS 6728 specifications.

[Measurement of dimensional variability]

The polymer film stored in a desiccator was cut into a dish-shaped sample with a diameter of 6 mm, and the sample was sandwiched between a pair of aluminum disks (with a diameter of 6 mm) to obtain a test sample. Put the test sample into a thermomechanical analyzer (model: TMA Q400, purchased from TA Instruments), and test the dimensional variability of the polymer film sample under the following conditions: use an expansion probe with a diameter of 2.8 mm Needle (expansion probe); force is set to 1.0 N; and the temperature is increased from 25°C to 145°C, and the heating rate is 10°C/min.

[Evaluation of surface roughness Rz value]

The surface roughness Rz value is measured using a roughness tester (model: SE 300, purchased from Kosaka Laboratory Ltd.) and measured in accordance with JIS B 0601 (1994). First, cut the polymer film into a size of 8 cm×30 cm as a test sample. Set the measurement conditions as follows: the vertical magnification is set to automatic, the horizontal magnification is set to 25 mm/λ _c , and the cut off distance is set to 2.5 mm (that is, calculated every 2.5 mm Once), the evaluation length is seven times the cut-off distance, the reference length is set to 17.5 mm, and the measurement direction is the machine direction.

[Bubble residual test and edge degumming test]

The laminated glass was cut to provide 20 test samples with a width of 150 mm and a length of 300 mm. Place the test sample vertically and maintain it in an environment with a temperature of 50°C and a relative humidity of 95% for 28 days. Afterwards, the test sample was visually observed for edge degumming and bubbles remaining, wherein the bubbles refer to bubbles that exist between the glass and the polymer film and are not in contact with external air. The evaluation criteria of the air bubble test are as follows: if there are no air bubbles remaining in any of the 20 test samples, the record is "◎", which means that the air bubble test result is excellent; if there are less than 3 of the 20 test samples The test sample has air bubbles remaining, and the record is "○", which means that the air bubble test result is good; if 3 to 5 test samples out of 20 test samples have air bubbles, the record is "△", which means the air bubble test result is not good ; And if more than 5 of the 20 test samples have air bubbles remaining, the record is "×", which means that the air bubble test result is extremely poor. The evaluation criteria of the edge degumming test are as follows: if none of the 20 test samples has edge degumming, the record is "◎", which means the edge degumming test is passed; and if there is at least one test sample in the 20 test samples There is edge degumming, recorded as "×", which means that the edge degumming test has not passed.

3.2. List of raw material information used in Examples and Comparative Examples

Table 1: List of raw material information Raw material model or abbreviation Description and source of purchase PVB Poly(vinyl butyral), purchased from Changchun Petrochemical Co., Ltd. 3GO Plasticizer, triethylene glycol bis(2-ethylhexanoate)

3.3. Preparation and quality testing of polymer film

According to the ratios shown in Tables 2-1 to 2-2, the polymer films of Examples 1 to 7 and Comparative Examples 1 to 7 were prepared, and the preparation methods are described as follows. First, mix PVB and 3GO according to the proportions shown in Tables 2-1 to 2-2 to obtain a mixture. After kneading the mixture for 15 minutes at 120°C with a rotation speed of 35 rpm, it is cooled to the chamber. Warm to obtain a PVB composition. Then, the PVB composition is placed in a hot press, and hot-compression bonding is performed at 150°C and a pressure of 3 kg for 3 minutes to obtain a polymer film.

Afterwards, if necessary, a pressing machine is used to mechanically press the two surfaces of the polymer film to obtain the desired surface roughness Rz value. The mechanical pressing conditions are as follows: the pressing wheel temperature is 120°C to 140°C, the pressing wheel pressure is 4 bar to 8 bar, and the linear speed of the polymer film passing between the pressing wheel is 9 m/min to 11 m/min .

According to the measurement method described above, measure the molecular weight distribution, hydroxyl content and viscosity of PVB of Examples 1 to 7 and Comparative Examples 1 to 7, as well as the thickness of the polymer film, the surface roughness Rz value, 45°C to 100° C dimensional variability and 100°C to 135°C dimensional variability, the results are shown in Table 2-1 to Table 2-2.

Table 2-1: Composition and properties of PVB and polymer films of Examples 1-7 unit Example 1 2 3 4 5 6 7 PVB Parts by weight 100 100 100 100 100 100 100 3GO Parts by weight 38.43 39.68 38.78 39.04 39.16 41.14 41.42 The thickness of the polymer film Mm 0.789 0.776 0.783 0.778 0.777 0.773 0.776 Rz of polymer film Micron 40.1 31.2 53.5 46.2 38.4 41.1 44.5 45°C to 100°C dimensional variability of polymer film Micron 36.20 28.76 43.21 31.00 33.63 34.12 30.69 100°C to 135°C dimensional variability of polymer film Micron 194.10 198.40 223.30 210.40 221.20 218.10 214.80 Viscosity of PVB cps 82 99 77 98 88 92 104 The hydroxyl content of PVB weight% 19.4 19.4 18.6 19.4 18.9 18.7 19.3 Molecular weight of PVB (Mw) Dalton 190982 207593 186573 181365 185764 195723 195434 The content of polymers with a molecular weight of >50,000 in PVB 13.7 mole% 13.5 mole% 15.7 mole% 14.4 Mole% 16.2 Mole% 16.5 mole% 14.3 Mole% The polymer content of PVB with a molecular weight> 800,000 6.3 mol% 5.4 mole% 6.1 mol% 4.7 mole% 4.5 mol% 5.2 mol% 6.1 mol% Pattern formation method of polymer film Mechanical pressed flower Mechanical pressed flower Mechanical pressed flower Mechanical pressed flower Mechanical pressed flower Mechanical pressed flower Mechanical pressed flower

Table 2-2: Composition and properties of PVB and polymer films of Comparative Examples 1-7 unit Comparative example 1 2 3 4 5 6 7 PVB Parts by weight 100 100 100 100 100 100 100 3GO Parts by weight 40.20 39.73 45.20 37.40 41.82 39.34 39.21 The thickness of the polymer film Mm 0.781 0.785 0.777 0.784 0.778 0.779 0.776 Rz of polymer film Micron 28.00 60.20 40.10 39.43 40.20 44.21 42.30 45°C to 100°C dimensional variability of polymer film Micron 34.35 35.44 56.32 15.32 55.00 17.43 54.20 100°C to 135°C dimensional variability of polymer film Micron 226.20 244.21 273.20 223.23 222.40 212.19 242.19 Viscosity of PVB cps 91 86 75 112 67 113 95 The hydroxyl content of PVB weight% 18.9 18.3 17.8 20.2 18.1 19.8 19.6 Molecular weight of PVB (Mw) Dalton 185698 183948 194532 196437 198287 190.87 182312 The content of polymers with a molecular weight of >50,000 15.6 mole% 16.3 mole% 17.9 mole% 13.5 mole% 17.9 mole% 13.5 mole% 19.5 mole% The polymer content of PVB with a molecular weight> 800,000 6.5 mole% 4.7 mole% 4.5 mol% 5.6 mole% 4.4 mol% 5.8 mole% 3.2 Mole% Pattern formation method of polymer film Melt fracture Melt fracture Mechanical pressed flower Mechanical pressed flower Mechanical pressed flower Mechanical pressed flower Mechanical pressed flower

3.4. Preparation and property evaluation of laminated glass

The polymer films of Examples 1 to 7 and Comparative Examples 1 to 7 were used to prepare laminated glass. First, prepare two clean and transparent float glass sheets (length 300 mm, width 150 mm, thickness 2 mm to 4 mm), and then combine the polymer films of Examples 1 to 7 and Comparative Examples 1 to 7 They are sandwiched between two transparent float glass sheets to obtain a laminate. Put the laminate into a vacuum bag and vacuum at a temperature of 20°C to 30°C (vacuum degree>500 mmHg (mmHg)) for at least 10 minutes, then put the vacuum bag containing the laminate into heating In the furnace, slowly increase the temperature of the heating furnace from 60°C to 130°C within at least 30 minutes, and then take out the vacuum bag from the heating furnace to complete the pre-compression bonding. Place the pre-compressed laminate in an autoclave at a pressure of 13 bar and a temperature of 135°C for 120 minutes, and then cool to room temperature to obtain a laminated glass.

The laminated glasses of Examples 1 to 7 and Comparative Examples 1 to 7 were subjected to bubble residue test and edge degumming test according to the method described above, and the results are recorded in Tables 3-1 and 3-2.

Table 3-1: Properties of laminated glass of Examples 1 to 7 Example 1 2 3 4 5 6 7 Bubble residue test ○ ◎ ◎ ◎ ◎ ◎ ○ Edge degumming test ◎ ◎ ◎ ◎ ◎ ◎ ◎

Table 3-2: Properties of laminated glass of Comparative Examples 1-7 Comparative example 1 2 3 4 5 6 7 Bubble residue test X △ X X X X X Edge degumming test ◎ ◎ X ◎ X ◎ X

As shown in Table 3-1, the laminated glass made from the polymer film of the present invention can obtain excellent and good results in the bubble residue test without edge degumming. The bubble residue test results are excellent and can pass the edge degumming test. . In particular, Examples 1 to 7 show that under different plasticizer content, PVB hydroxyl content, PVB molecular weight, and dimensional variability from 100°C to 135°C, as long as the polymer film has a size of 45°C to 100°C The variability and surface roughness Rz are within the specified range, and the prepared laminated glass can meet the requirements of obtaining excellent and good results in the bubble residue test and no edge degumming.

In contrast, as shown in Table 3-2, the laminated glass made from the polymer film that does not belong to the present invention cannot meet the requirements of obtaining excellent and good results in the bubble residue test without edge degumming. In particular, Comparative Examples 1 to 7 show that regardless of the plasticizer content, PVB hydroxyl content, PVB molecular weight, and 100°C to 135°C dimensional variability, as long as the polymer film has a 45°C to 100°C dimensional variability And the surface roughness Rz is not within the specified range of the present invention at the same time, the prepared laminated glass cannot meet the requirements of obtaining excellent and good results in the bubble residue test without edge degumming.

The above-mentioned embodiments are merely illustrative to illustrate the principle and effects of the present invention, and to illustrate the technical features of the present invention, and are not intended to limit the scope of protection of the present invention. Any changes or arrangements that can be easily made by those skilled in the art without departing from the technical principles and spirit of the present invention fall within the claimed scope of the present invention. Therefore, the protection scope of the present invention is as listed in the appended patent scope.

no

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Claims (14)

A polymer film comprising polyvinylacetal (polyvinylacetal), wherein: The polymer film has a 45°C to 100°C dimensional variability of 20 microns to 50 microns; and At least one surface of the polymer film has a surface roughness Rz value of 30 micrometers to 55 micrometers. The polymer film according to claim 1, wherein the polymer film has a 45°C to 100°C dimensional variability of 28 micrometers to 44 micrometers, and at least one surface of the polymer film has a diameter of 31 micrometers to 54 micrometers. Surface roughness Rz value. The polymer film according to claim 1, wherein the two surfaces of the polymer film independently have a surface roughness Rz value of 30 micrometers to 55 micrometers. The polymer film according to claim 1, wherein the polyvinyl acetal is selected from the following group: poly(vinyl formal), poly(vinyl formal), poly(vinyl formal), poly(vinyl formal), poly(vinyl formal), poly(vinyl formal), poly(vinyl formal), poly(vinyl formal), poly(vinyl formal), poly(vinyl formal), poly(vinyl formal) (Vinyl butyral), poly(vinyl butyral), poly(vinyl hexanal), and combinations thereof. The polymer film according to claim 1, wherein the hydroxyl content of the polyvinyl acetal is 13% to 25% by weight. The polymer film according to claim 1, wherein the weight average molecular weight (Mw) of the polyvinyl acetal is 150,000 daltons to 250,000 daltons. The polymer film according to claim 1, wherein in the polyvinyl acetal, the content of the polyvinyl acetal having a molecular weight of less than 50,000 daltons is 10 mol% to 20 mol%. The polymer film according to claim 1, wherein in the polyvinyl acetal, the content of the polyvinyl acetal with a molecular weight higher than 800,000 Daltons is 1 mol% to 10 mol%. The polymer film according to any one of claims 1 to 8, further comprising a plasticizer. The polymer film according to claim 9, wherein the content of the plasticizer is 30 to 60 parts by weight based on 100 parts by weight of polyvinyl acetal. The polymer film according to any one of claims 1 to 8, which has a thickness of 0.5 mm to 1.5 mm. The polymer film according to any one of claims 1 to 8, which is a multilayer film. The polymer film according to any one of claims 1 to 8, further comprising additives selected from the following group: dyes, pigments, stabilizers, antioxidants, flame retardants, infrared absorbers, infrared blocking agents, ultraviolet rays Absorbents, UV stabilizers, lubricants, dispersants, surfactants, chelating agents, coupling agents, bonding agents, adhesion control agents, and combinations thereof. A laminated glass comprising a first glass sheet, a second glass sheet, and a polymerization as described in any one of claims 1 to 13 arranged between the first glass sheet and the second glass sheet物膜。 The film.