Polyurethane-based elastomer anode material for anodic bonding

Abstract

The invention discloses a polyurethane-based elastomer anode material suitable for anodic bonding, which is prepared by the following steps: preparing a prepolymer component A based on oligomer polyol, diisocyanate and a conductive polymer, mixing and stirring a chain extender, a cross-linking agent, a catalyst and the conductive polymer to prepare a prepolymer component B, and uniformly mixing the prepolymer component A and the prepolymer component B to prepare the polyurethane-based elastomer anode material suitable for anodic bonding. And pouring the mixture into a mold coated with a release agent for curing to obtain the polyurethane-based elastomer anode material. The polyurethane-based elastomer anode material disclosed by the invention can be bonded with a glass anode, so that the problem of permanent connection between an intermediate polymer and glass on two sides of laminated glass is solved.

Description

TECHNICAL FIELD

[0001] The present application belongs to the field of laminated glass, and particularly relates to a high-performance laminated glass with an elastic interlayer connected to two sides of glass by anodic bonding. BACKGROUND

[0002] Laminated glass is widely used in the fields of automobile, high-rise building door and window, glass curtain wall, sightseeing elevator passage, glass guardrail, indoor partition, lighting roof and other places or parts with high safety performance requirements as a material with safety, energy saving and environmental protection functions. Ordinary glass will break under general impact, and tempered glass will break under greater force impact. Once broken, long and sharp fragments or fine particles without sharp corners will be produced, which will pose a great threat to personal safety. Laminated glass is obtained by placing a polymer film between two or more layers of glass, combining the toughness of the polymer film and the hardness of the glass together, and then processing by high temperature and high pressure. The production process of laminated glass usually includes dry hot pressing process and wet grouting process. The dry hot pressing process is to firmly bond glass and interlayer material together by applying high temperature and pressure. The interlayer materials used in the dry laminated process include PU, PVB, EVA, SGP and the like. The wet grouting process is to fill liquid polymer material into the gap between two pieces of glass, and then to solidify and bond with the glass surface by sunlight exposure or high temperature baking.

[0003] With the increase of service life, the delamination and debonding defects will gradually appear. Common quality problems are point defects and debonding, which result in poor appearance transparency of the laminated glass, visual obstruction, affect the appearance beauty, and even affect the safety. Good bonding between glass and adhesive layer is a necessary condition to ensure the integrity and safety of laminated glass. Debonding not only reduces the transparency of laminated glass, but also causes certain safety hazards. The "adhesive layer" of the current "adhesive" technology of laminated glass is prone to aging and falling off under the environment of high temperature, high humidity and sunlight exposure.

[0004] Anodic bonding is a process of interconnecting materials by forming chemical bonds through electrochemical reactions between different material interfaces under the coupling of multiple fields. The traditional cathode material is usually glass, and the anode material is metal or semiconductor silicon. Anodic bonding can minimize the concentrated thermal stress caused by the mismatch of the thermal expansion coefficients of different materials. Anodic bonding is simple to operate, does not require intermediate filler assistance, and has high connection strength and good sealing performance. If an elastic anode material that can be anodically bonded with glass can be developed, it will have a revolutionary impact on the connection performance between the interlayer polymer layer and the two sides of glass of laminated glass. SUMMARY

[0005] The present application aims to develop a polyurethane-based elastomer anode material suitable for anodic bonding, which can be permanently connected with glass through anodic bonding.

[0006] The technical solution of the present application is as follows: a polyurethane-based elastomer anode material for anodic bonding, comprising the following steps: Preparation of prepolymer A component and prepolymer B component; Pouring the mixture of the prepolymer A component and the prepolymer B component into a mold coated with a release agent for curing to obtain the polyurethane-based elastomer anode material.

[0007] Further, the preparation process of the prepolymer A component comprises: vacuum dehydration of metered oligomer polyol PTMG or PPG 20-60 parts by mass at 100-110°C for 0.5-1 hour. Then, cool down to 30-50°C, add diisocyanate MDI or IPDI 8-20 parts by mass, after natural temperature rise stops, slowly heat to 70-80°C, and keep warm for 2 hours to obtain the prepolymer. Add conductive polymer polyaniline, or polythiophene, or polypyrrole 6-18 parts by mass in the prepolymer, stir for 0.5-1 hour, and then seal and stand for 3-6 hours.

[0008] Further, the preparation process of the prepolymer B component comprises: vacuum dehydration of chain extender MOCA or BDO 3-6 parts by mass, crosslinking agent TMP 3-6 parts by mass at 100-110°C for 1 hour, add appropriate amount of catalyst DBTL 2-5 parts by mass, conductive polymer polyaniline, or polythiophene, or polypyrrole 3-9 parts by mass, and mix uniformly.

[0009] Further, the functionality of the chain extender BDO or MOCA and the crosslinking agent TMP is different, and the branching degree of the product can be controlled by adjusting the ratio of the two.

[0010] Further, the NCO% of the prepolymer A component is set to 8, and the chain extension coefficient is 0.9.

[0011] Further, the mixture process of the prepolymer A component and the prepolymer B component comprises: rapid mixing of the prepolymer A component and the prepolymer B component, and rapid stirring for 2-4 minutes, and then defoaming for 30-90 seconds; pouring the mixture into a room temperature mold coated with a release agent, and curing at room temperature for 7-10 days.

[0012] Further, a polyurethane-based elastomer anode material suitable for anodic bonding is prepared by the above preparation method, which comprises a mixed product of prepolymer and conductive polymer, and a chain extension system and conductive polymer synergistic complex.

[0013] Another technical solution of the present application: an application of the polyurethane-based elastomer anode material for anodic bonding, the polyurethane-based elastomer anode material for anodic bonding is used for anodic bonding, comprising: surface cleaning a polyurethane-based elastomer anode material sheet and a glass sheet respectively, and then stacking the two together and placing them in an anodic bonding machine for anodic bonding experiment.

[0014] The polyurethane-based elastomer anode material for anodic bonding prepared by the process has good comprehensive performance and can successfully realize anodic bonding with a glass sheet.

[0015] Compared with the prior art, the specific advantages are as follows: (1) The polyurethane-based elastomer anode material has good mechanical properties, high light transmittance, good heat resistance, and in addition, safety, sound insulation, security, shock resistance, sunshade and other properties.

[0016] (2) The polyurethane-based elastomer anode material can realize anodic bonding connection with glass.

[0017] (3) Due to the use of prepolymer method, the pouring system has low viscosity, which is beneficial to defoaming and can obtain a material with high surface flatness.

[0018] (4) The present application first uses polyurethane material as an anode material for anodic bonding, further widening the application range of anodic bonding. BRIEF DESCRIPTION OF DRAWINGS

[0019] Figure 1 Figure 1 is a scanning electron microscope image of the anodic bonding cross section of Example 1 of the present application; Figure 2 Figure 2 is a scanning electron microscope image of the anodic bonding cross section of Example 2 of the present application; Figure 3 Figure 3 is a scanning electron microscope image of the anodic bonding cross section of Example 3 of the present application. DETAILED DESCRIPTION

[0020] The present application will be further described in detail below in combination with examples, but the protection scope of the present application is not limited to these examples. In the following examples, there is no special limitation on the source of all raw materials, and the raw materials used are commercially available. EXAMPLE

[0021] The present embodiment provides a preparation method of a polyurethane-based elastomer anode material for anodic bonding, comprising the following steps: (1) A component: measured PPG mass parts 40 parts are added to a three-necked flask, vacuum dehydration at 105°C for 1 hour. Then cool down to 40°C, add MDI mass parts 12 parts, after natural temperature rise stops, slowly heat to 70°C, keep temperature for 2 hours to get prepolymer. Add conductive polymer polypyrrole mass parts 10 parts in the prepolymer, stir for 0.5 hours, then seal and stand for 3 hours.

[0022] (2) B component: chain extender BDO mass parts 3 parts, crosslinking agent TMP mass parts 4 parts are vacuum dehydrated at 105°C for 1 hour, add appropriate amount of catalyst DBTL mass parts 2 parts, conductive polymer polypyrrole mass parts 5 parts are uniformly mixed and stirred.

[0023] (3) quickly mix A component and B component, and quickly stir for 2 minutes, then defoam for 60 seconds; quickly pour the mixture into a room temperature mold coated with a release agent, and cure at room temperature for 7 days.

[0024] (4) the prepared 2mm thick polyurethane-based elastomer anode material sheet and 2mm thick glass sheet are respectively surface cleaned, then nitrogen dried, and then stacked together and placed in an anode bonding machine for an anode bonding experiment, and the polyurethane-based elastomer anode material sheet and the glass sheet are connected. Embodiment

[0025] The embodiment provides a preparation method of a polyurethane-based elastomer anode material for anode bonding, comprising the following steps: (1) A component: measured TMPG mass parts 45 parts are added to a three-necked flask, vacuum dehydration at 110°C for 1 hour. Then cool down to 50°C, add IPDI mass parts 13 parts, after natural temperature rise stops, slowly heat to 70°C, keep temperature for 2 hours to get prepolymer. Add conductive polymer polypyrrole mass parts 10 parts in the prepolymer, stir for 0.5 hours, then seal and stand for 3 hours.

[0026] (2) B component: chain extender BDO mass parts 4 parts, crosslinking agent TMP mass parts 4 parts are vacuum dehydrated at 105°C for 1 hour, add appropriate amount of catalyst DBTL mass parts 2 parts, conductive polymer polypyrrole mass parts 5 parts are uniformly mixed and stirred.

[0027] (3) quickly mix A component and B component, and quickly stir for 2 minutes, then defoam for 50 seconds; quickly pour the mixture into a room temperature mold coated with a release agent, and cure at room temperature for 7 days.

[0028] (4) the prepared 2mm thick polyurethane-based elastomer anode material sheet and 3mm thick glass sheet are respectively surface cleaned, then nitrogen dried, and then stacked together and placed in an anode bonding machine for an anode bonding experiment, and the polyurethane-based elastomer anode material sheet and the glass sheet are connected. Embodiment

[0029] The embodiment provides a preparation method of a polyurethane-based elastomer anode material for anodic bonding, comprising the following steps: (1) A component: a metered quantity of 45 parts of TMPG is added into a three-necked flask, vacuum dehydration is carried out at 110 DEG C for 1 hour. Then, the temperature is lowered to 45 DEG C, 15 parts of IPDI is added, after natural temperature rising is stopped, slow heating is carried out to 70 DEG C, and after 2 hours of temperature maintaining reaction, a prepolymer is obtained. 10 parts of conductive polymer polythiophene is added into the prepolymer, stirring is carried out for 0.5 hours, and then sealing and standing are carried out for 3 hours.

[0030] (2) B component: 3 parts of chain extender BDO, 4 parts of crosslinking agent TMP are vacuum dehydrated at 105 DEG C for 1 hour, 3 parts of appropriate catalyst DBTL, 4 parts of conductive polymer polypyrrole are uniformly mixed and stirred.

[0031] (3) The A component is rapidly mixed with the B component, rapid stirring is carried out for 2 minutes, and then defoaming is carried out for 50 seconds; the mixture is rapidly poured into a room temperature mold coated with a release agent, and room temperature curing is carried out for 7 days.

[0032] (4) The prepared 2mm-thick polyurethane-based elastomer anode material sheet and 3mm-thick glass sheet are respectively subjected to surface cleaning, and then nitrogen blowing is carried out, the two are stacked together and placed in an anodic bonding machine to carry out an anodic bonding experiment, and the polyurethane-based elastomer anode material sheet and the glass sheet form connection.

[0033] The polyurethane-based elastomer anode material obtained in the above embodiment 1-3 is tested, and the test results are shown in Table 1.

[0034] Table 1 Performance test Examples T 600 / %]]> % Elongation at break Tensile strength / MPa Example 1 89 412 1.1 Example 2 90 385 1.7 Example 3 88 364 1.8 The anodic bonding cross section scanning of the polyurethane-based elastomer anode material obtained in the above embodiment 1-3 is carried out, and the scanning results are shown in Figures 1-3 , and the middle connecting layer can be clearly seen.

[0035] The above only describes the preferred embodiments of the present application, and it should be noted that, for ordinary skilled in the art, without departing from the principles of the present application, a number of improvements and refinements can be made, and these improvements and refinements should be regarded as the protection scope of the present application.

Claims

1. A method for producing a polyurethane-based elastomeric anode material, characterized by, The method comprises the following steps: Preparation of prepolymer A component and prepolymer B component; Pouring the mixture of prepolymer A component and prepolymer B component into a mold coated with a release agent for curing to obtain a polyurethane-based elastomer anode material.

2. The method for preparing a polyurethane-based elastomer anode material according to claim 1, wherein: The preparation process of the prepolymer A component comprises: vacuum dehydration of 20-60 parts by mass of an oligomeric polyol PTMG or PPG at 100-110°C for 0.5-1 hour. Then, the temperature is lowered to 30-50°C, 8-20 parts by mass of diisocyanate MDI or IPDI is added, after the natural temperature rise stops, the temperature is slowly raised to 70-80°C, and the prepolymer is obtained after 2 hours of incubation. 6-18 parts by mass of conductive polymer polyaniline, or polythiophene, or polypyrrole is added to the prepolymer, stirred for 0.5-1 hour, and then sealed and placed for 3-6 hours.

3. The method for preparing a polyurethane-based elastomer anode material according to claim 1, wherein: The preparation process of the prepolymer B component comprises: vacuum dehydration of 3-6 parts by mass of chain extender MOCA or BDO and 3-6 parts by mass of crosslinking agent TMP at 100-110°C for 1 hour, and uniformly mixing 2-5 parts by mass of appropriate catalyst DBTL, 3-9 parts by mass of conductive polymer polyaniline, or polythiophene, or polypyrrole.

4. The method for preparing a polyurethane-based elastomer anode material according to claim 1, characterized in that: The chain extender BDO or MOCA and the crosslinking agent TMP have different functionalities, and the branching degree of the product can be controlled by adjusting the ratio of the two.

5. The method for preparing a polyurethane-based elastomer anode material according to claim 2, characterized in that: The NCO% of the prepolymer A component is set to 8, and the chain extension coefficient is 0.

9.

6. The method for preparing a polyurethane-based elastomer anode material according to claim 1, characterized in that: The mixture process of the prepolymer A component and the prepolymer B component comprises: rapidly mixing the prepolymer A component and the prepolymer B component, and rapidly stirring for 2-4 minutes, and then defoaming for 30-90 seconds; rapidly pouring the mixture into a room temperature mold coated with a release agent, and curing at room temperature for 7-10 days.

7. A polyurethane-based elastomeric anode material suitable for anodic bonding, characterized in that, The product obtained by the method of any one of claims 1-6, comprising a mixture of prepolymer and conductive polymer, a chain extension system and a synergistic complex of conductive polymer.

8. A polyurethane-based elastomeric anode material suitable for anodic bonding according to claim 7, characterized in that, The product obtained by the method of any one of claims 1-7.

9. Use of a polyurethane-based elastomeric anode material suitable for anodic bonding, characterized in that A polyurethane-based elastomer anode material sheet suitable for anode bonding according to claim 7 or 8 and a glass sheet are respectively surface cleaned, and then stacked together and placed in an anode bonding machine for anode bonding experiment, and the polyurethane-based elastomer anode material sheet and the glass sheet are connected.

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