Production process of tempered laminated glass

By employing rigorous raw material screening, a three-zone gradient tempering process, precise PVB interlayer lamination, and a staged curing process in an autoclave, the problem of low production efficiency in tempered laminated glass has been solved, enabling the efficient production of high-quality tempered laminated glass.

CN120792291APending Publication Date: 2025-10-17HUIZHOU QIANLU GLASS TECHNOLOGY CO LTD

Patent Information

Application Number
CN202510901707.8
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-07-01
Publication Date
2025-10-17

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Abstract

The invention discloses a production process of tempered laminated glass, which belongs to the technical field of tempered glass, and comprises the following steps: strictly screening raw sheets, carrying out three-zone gradient tempering, namely, mutually combining 680-700 DEG C temperature zone temperature control and 8-12kPa gradient wind pressure quenching, and precisely compounding by using a PVB interlayer to obtain the tempered laminated glass. 23 DEG C / 30% RH pre-balancing, 0.5 mm vacuum positioning and 120-140 DEG C rolling initial pressing are combined, and then high-pressure kettle staged curing, namely, the process of heat preservation for 120 minutes at 1.2 MPa / 135 DEG C and the process of gradient cooling at the temperature smaller than or equal to 15 DEG C / h are combined, so that the finally prepared tempered glass product has high optical performance, namely distortion smaller than or equal to 0.1 mm / mm, high impact resistance, namely no penetration in 1m steel ball falling and excellent weather resistance; degumming is avoided in the environment of 85 DEG C / 85% RH / 500 h, and accurate control over the whole process from materials to finished products is achieved. Therefore, the production process of the tempered laminated glass solves the technical problem of how to improve the production efficiency of the tempered laminated glass.
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Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of toughened glass, and particularly relates to a production process of toughened laminated glass. BACKGROUND

[0002] Glass is a common and widely used building decoration material, which can effectively reduce the self-weight of the building and enhance the decoration aesthetics of the building. With the improvement of people's living standards, the development of science and technology and the progress of society, people's requirements for glass are increasingly diversified, functional and green. Various functional glass deep processing products, such as frosted glass, colored glaze glass, coated glass, low-emissivity glass and embossed glass, are gradually favored by people.

[0003] However, glass is a brittle material, which is easy to endanger personal safety when broken, especially the glass of high-rise buildings is more dangerous. The strength of brittle materials depends largely on the surface structure. The surface of glass looks complete and smooth, but in fact there are a large number of micro-cracks. The micro-cracks are expanded under the action of tensile stress, and then broken from the surface. Therefore, if the influence of these surface micro-cracks can be eliminated, the tensile strength can be significantly improved. The tempering method is an effective method to eliminate the influence of surface micro-cracks, which makes the surface layer of glass under strong compressive stress. Only when the tensile stress acting on the surface layer of glass exceeds the compressive stress that it can bear, the glass can be broken. Therefore, the tempered glass can improve the compressive strength.

[0004] Therefore, the Chinese patent document with the publication number CN108215431B discloses a manufacturing method of tempered laminated glass, which comprises the following steps: cutting, edging and cleaning the first glass substrate and the second glass substrate used for manufacturing the tempered laminated glass; determining the placement position and sequence of the glass substrates; cleaning the first glass substrate, laying the intermediate adhesive film on the first glass substrate, and then placing the second glass substrate; the bending directions of the first glass substrate and the second glass substrate are the same; sending the first glass substrate and the second glass substrate after splicing into a flat press for preheating and prepressing; sending the first glass substrate and the second glass substrate after prepressing into an autoclave for heat preservation and pressure preservation, so that the first glass substrate, the second glass substrate and the intermediate adhesive film are completely bonded together. The technical solution disclosed by the patent document is beneficial to improving the production yield of double-tempered laminated glass, reducing rework, saving energy and improving efficiency.

[0005] However, the above disclosed tempered laminated glass production method still has the technical problem of insufficient production efficiency. Specifically, in actual production, improving the production efficiency of tempered laminated glass needs to start from three aspects of process optimization, intelligent control and equipment upgrading: first, optimize the tempering process parameters, such as extending the heating time of hole glass by 2.5%-5%, adjusting the placement direction of sharp corner glass to reduce deformation; second, introduce an intelligent temperature control system to realize precise regulation and control in multiple areas, reduce energy consumption through frequency conversion technology, and reduce downtime combined with predictive maintenance; finally, upgrade the automatic production line, replace the intermittent equipment with a continuous tunnel furnace, integrate ERP and MES systems to realize the linkage of order and production data, which can reduce 30% of manual intervention and improve the flow speed. In addition, for special products such as embossed glass, the heating strategy needs to be adjusted to ensure that the texture surface faces up and the heating time of the thickest area is extended to ensure uniformity. SUMMARY

[0006] Therefore, it is necessary to provide a production process of tempered laminated glass for improving the production efficiency of tempered laminated glass.

[0007] A production process of tempered laminated glass, comprising the following steps: S1: raw sheet selection and pretreatment: selecting float glass or ultra-white glass as the base material, and controlling the iron content of the ultra-white glass to be not more than 0.015% and the light transmittance of the float glass to be not less than 91.5%; then grouping and managing the thickness of the base material, controlling the deviation of the base material in the same batch to be not more than 0.1mm; then cleaning the base material, using a combination of deionized water and ultrasonic cleaning to remove particles on the surface of the base material, controlling the diameter of the residues on the surface of the base material to be not more than 5μm; finally, laser cutting and edge grinding the base material according to the preset size; S2: tempering treatment: the temperature control in the heating stage is 650-700℃, and the control interval in the heating stage is divided into three zones for separate temperature control, i.e. preheating zone 680℃±5℃, soaking zone 700℃±3℃ and balance zone 690℃±5℃; in the quenching process, the wind pressure is controlled by gradient, such as 0-3 seconds, 8kPa; 3-6 seconds, 12kPa; 6 seconds later, reduced to 5kPa; during stress detection, the surface compressive stress of the product is controlled to be ≥90MPa, and the stress layer depth is ≥0.1t, wherein t is the thickness of the glass; S3: laminated composite process: in the PVB film pretreatment, the temperature is controlled to be 23±2℃ and the humidity is controlled to be 30±5% for 24 hours; in the sheet positioning process, the vacuum chuck clamp is used to ensure the positioning accuracy within 0.5mm; the initial pressure exhaust is controlled to be 120-140℃, the pressure is controlled to be 0.6-0.8MPa, and the speed is controlled to be 2-3m / min; S4: autoclave curing: in the heating stage, the temperature is raised to 135±5℃ at a rate of 8-10℃ / min under a pressure of 1.0-1.2MPa; in the holding stage, the temperature is maintained for 120min to make the PVB refractive index fully match the glass; in the cooling stage, the temperature is lowered to below 50℃ at a rate of ≤15℃ / h before the autoclave is opened; S5: after the completion of the production of the tempered laminated glass, the quality of the glass is monitored according to the preset quality detection standard.

[0008] Further, in step S1, when the substrate is laser cut, a CO2 laser cutting machine with a wavelength of 10.6μm is used for cutting; the kerf taper of the substrate is controlled to be 0.02mm / m, and the cutting speed and power relationship is controlled according to the following formula one: Formula one: P=0.8×e 0.05v Wherein, v is the cutting speed, unit mm / s; P is the power, unit kW.

[0009] Further, in step S1, when the substrate is laser cut, a CO2 laser cutting machine with a wavelength of 10.6μm is used for cutting; the kerf taper of the substrate is controlled to be 0.02mm / m, and the cutting speed and power relationship is controlled according to the following formula two: Formula two: P=0.8×e 0.05v +0.02ΔT; Wherein, v is the cutting speed, unit mm / s; P is the power, unit kW; ΔT is the environmental temperature change, unit ℃.

[0010] Further, in step S1, after the laser cutting of the substrate is completed, the edge grinding process is as follows: 45° chamfer plus circular arc transition composite machining, and then, three-stage diamond grinding wheels with specifications of 400#, 800# and 1500# are used for step-by-step polishing.

[0011] Further, in step S2, the tempering process parameters are optimized as follows: temperature field control: a PID three-closed-loop temperature control system is used to allow the heating elements to be independently adjusted in zones, and the thermocouple spacing is ≤150mm.

[0012] Further, in step S2, the tempering process parameters are optimized as follows: quenching kinetics: the air nozzle array is designed as follows: upstream zone: Φ3mm hole, spacing 15mm, inclination 30°, downstream zone: Φ5mm hole, spacing 20mm, inclination 45°.

[0013] Further, in step S2, the tempering process parameters are optimized as follows: stress testing: a SCALP-05 stress meter is used, and the detection point density is ≥9 points / m².

[0014] Further, in step S3, a pre-humidity treatment curve is adopted in the PVB film treatment to realize segmented control: 0-4h: 25%RH±2%, 4-12h: 30%RH±1%, 12-24h: 28%RH±1%.

[0015] Further, in step S3, the parameters of the lamination positioning system are as follows: machine vision assisted positioning, CCD resolution 0.01mm / pixel, and repeated positioning accuracy ±0.05mm.

[0016] In summary, the production process of the tempered laminated glass of the present application realizes the full-process precise control from the material to the finished product, and the prepared tempered glass product has high optical performance (distortion ≤0.1mm / mm), strong impact resistance (1m steel ball drop without penetration), and excellent weather resistance (no delamination in 85℃ / 85%RH / 500h environment), and realizes the technical problem of how to improve the production efficiency of the tempered laminated glass. DETAILED DESCRIPTION

[0017] To make the above objectives, features and advantages of the present application more obvious and easy to understand, the specific embodiments of the present application will be described in detail below. In the following description, a large number of specific details are set forth in order to facilitate a full understanding of the present application. However, the present application can be implemented in many other ways different from those described herein, and those skilled in the art can make similar improvements without departing from the scope of the present application, so the present application is not limited to the specific embodiments disclosed below.

[0018] Specifically, the production process of the tempered laminated glass of the present application includes the following steps: S1: raw sheet selection and pretreatment: float glass or ultra-white glass is selected as the base material, and the iron content of the ultra-white glass is controlled to be not more than 0.015%, and the light transmittance of the float glass is controlled to be not less than 91.5%; then the thickness of the base material is grouped and managed, and the deviation of the base material in the same batch is controlled to be not more than 0.1mm; then the base material is cleaned by combining deionized water with ultrasonic cleaning to remove the particles on the surface of the base material, and the diameter of the residues on the surface of the base material is controlled to be not more than 5μm; finally, the base material is laser cut and edge ground according to the preset size; S2: toughening treatment: the temperature control in the heating stage is 650-700°C, and the temperature control in the heating stage is divided into three zones, namely: the preheating zone is 680°C±5°C, the soaking zone is 700°C±3°C, and the balance zone is 690°C±5°C; in the quenching process, the air pressure is controlled by gradient, such as: 0-3 seconds, 8kPa; 3-6 seconds, 12kPa; 6 seconds later, reduce to 5kPa; when stress testing, the surface compressive stress of the product is controlled to be greater than or equal to 90MPa, and the stress layer depth is greater than or equal to 0.1t, wherein t is the thickness of the glass; S3: interlayer composite process: in the PVB film pretreatment, the temperature is controlled at 23±2°C and the humidity is controlled at 30±5% for 24 hours; in the laminating positioning process, the vacuum chuck clamp is used to ensure the positioning accuracy within 0.5mm; the initial pressure is controlled at 120-140°C, the pressure is controlled at 0.6-0.8MPa, and the speed is controlled at 2-3m / min; S4: autoclave curing: in the heating stage, the temperature is increased to 135±5°C at a rate of 8-10°C / min under a pressure of 1.0-1.2MPa; in the pressure maintaining stage, the PVB refractive index is completely matched with the glass by maintaining for 120 minutes; in the cooling stage, the temperature is decreased to below 50°C at a rate of ≤15°C / h, and then the autoclave is opened; S5: after the production of the toughened laminated glass is completed, the quality of the glass is monitored according to the preset quality detection standard, such as: according to the standard of GB / T9963-2025, the optical distortion of the glass is controlled to be ≤0.1mm / mm; the impact resistance of the glass is controlled to be no penetration in the 1040g steel ball 1m drop test; the weather resistance test of the glass meets the storage for 500 hours in the environment of 85°C / 85%RH without delamination.

[0019] Specifically, in the foregoing production process of the toughened laminated glass, the following core advantages are provided: Material precise control: strictly selecting the base material with iron content≤0.015% and transmittance≥91.5% can ensure excellent optical performance of the final product; the thickness deviation of the same batch is≤0.1mm, which significantly improves the product uniformity. The use of ultrasonic wave combined with deionized water cleaning can effectively remove surface particles, so that the diameter of the residual particles is≤5μm, reducing the risk of interlayer bubbles.

[0020] Efficient toughening process: three-zone independent temperature control, namely preheating zone 680°C±5°C, soaking zone 700°C±3°C, and balance zone 690°C±5°C, which optimizes the heating uniformity and reduces thermal deformation. Gradient air pressure quenching, namely 8kPa→12kPa→5kPa gradient control, can make the surface compressive stress of the finished product glass≥90MPa / stress layer depth≥0.1t, which strengthens the mechanical strength and impact resistance of the final product.

[0021] Laminated composite stability: PVB film pre-equilibrium, that is, the control process of 23±2℃ / 30±5%RH / 24h can guarantee the stability of water content and avoid delamination in later period; the positioning accuracy of vacuum chuck reaches 0.5mm, which improves the alignment of lamination. The initial pressure parameter is optimized, that is, 120-140℃ / 0.6-0.8MPa / 2-3m / min, which can strengthen the exhaust effect and reduce the residual bubbles in the interface.

[0022] Curing process reliability: high-pressure kettle controls temperature in stages: the heating rate is 8-10℃ / min / 1.0-1.2MPa to 135±5℃, the holding time is 120 minutes, the cooling rate is ≤15℃ / h gradient cooling, which can effectively eliminate internal stress and ensure complete fusion of the glue layer.

[0023] Quality assurance system: optical distortion ≤0.1mm / mm, which meets the relevant standards of GB / T9963-2025, impact resistance, which has no penetration phenomenon in the test of 1040g steel ball 1m drop, weather resistance, which has no delamination phenomenon in the storage environment of 85℃ / 85%RH / 500h, so that the tempered laminated glass prepared by the application can fully meet the high-standard performance verification.

[0024] Further, in the step S1, when the substrate is laser cut, a CO2 laser cutting machine with a wavelength of 10.6μm can be used to cut the substrate, and the notch taper is controlled at 0.02mm / m, and the cutting speed and power are controlled according to the following formula one: Formula one: P=0.8×e 0.05v Wherein, v is the cutting speed, unit mm / s; P is the power, unit kW.

[0025] The above formula one describes the characteristic that the power increases exponentially with the cutting speed in the laser glass cutting process; the exponential growth relationship: power (P) and speed (v) are in exponential function relationship (e 0.05v ), which shows that when the speed increases, the power demand nonlinearly rises, for example: When V=0, P=0.8×e 0 =0.8kW, which is the basic power of laser cutting.

[0026] When V=10mm / s, e0.5≈1.648, P≈1.32kW.

[0027] When V=20mm / s, e l ≈2.718, P≈2.17kW, which means that speed doubling leads to a power growth of about 170%.

[0028] Specifically, the constant term 0.8kW represents the initial power, i.e. the minimum energy required for device startup or low-speed state; the exponential coefficient 0.05 / mm / s reflects the sensitivity of speed to power; the greater the value, the more significant the impact of speed change on power.

[0029] Physical mechanism: synergy of speed and power, energy density requirement, i.e. higher laser power is needed for high-speed cutting to input sufficient energy per unit time to overcome material heat capacity and achieve effective melting or evaporation; otherwise, the cutting depth is insufficient or the edge quality is poor. Thermal accumulation effect, i.e. heat is easy to accumulate at low speed, leading to material overheating defects; at high speed, the power needs to be exponentially increased to maintain thermal balance and avoid discontinuous cutting or micro-cracks.

[0030] Further, an environmental variable such as temperature ΔT can be introduced as dynamic compensation, so that the above formula one can be optimized to obtain the following formula two: Formula two: P=0.8×e 0.05v +0.02ΔT; Where v is the cutting speed, unit mm / s; P is the power, unit kW; ΔT is the environmental temperature change, unit ℃.

[0031] From formula two, the actual working condition adaptability can be enhanced. Experiments show that when the speed is 10-15mm / s, the power grows slowly, and the slope at this time is 0.15kW / (mm / s). If it exceeds this range, there will be defects of cost-effectiveness decline.

[0032] Further, an embodiment is as follows: When cutting 8mm super white glass with a transmittance ≥91.5%, calculate according to formula one as follows: Target speed V=12mm / s, calculate power: P=0.8×e0.05x12=0.8×e0.6≈0.8×1.822=1.46kW If burrs appear during actual cutting, the cutting speed can be reduced to V=8mm / s, and the power P≈1.19kW to improve the edge quality; this formula quantifies the speed-power trade-off mechanism and is a core parameter control method for achieving efficient and high-quality laser cutting.

[0033] Further, in the aforementioned step S1, after completing laser cutting on the substrate, the edge grinding process used is: 45° chamfering plus circular arc transition composite processing, and then using 400#, 800# and 1500# three-stage diamond grinding wheels for step-by-step polishing of the substrate.

[0034] Specifically, in the aforementioned step S2, the tempering process parameters are optimized as follows: Temperature field control: PID three-closed-loop temperature control system (heating element partition independent adjustment), thermocouple spacing ≤ 150 mm.

[0035] Quenching kinetics: The air nozzle array design is: upstream zone: Φ3mm hole, spacing 15mm, inclination 30°, downstream zone: Φ5mm hole, spacing 20mm, inclination 45°.

[0036] Stress test: Using SCALP-05 stress meter, detection point density ≥ 9 points / m².

[0037] Specifically, the core principle of tempering process parameter optimization is to control the uniformity of the temperature field and the quenching kinetics process, so that the gradient distribution of the glass surface stress and the accurate balance of the internal tension can be realized. The specific principle is as follows: 1. Temperature field control system principle PID three-closed-loop temperature control mechanism: Proportional link (P): According to the deviation of real-time detection temperature and set value of thermocouple, the partition heating element immediately adjusts the power linearly. Because the greater the deviation, the stronger the power compensation, so that the heating rate can be achieved ≥ 15℃ / min.

[0038] Integral link (I): Accumulate the historical deviation of partition temperature difference, such as continuous low temperature in a certain area, continuously increase the heating power of the area, eliminate steady-state error, and make the temperature control accuracy reach ±2℃.

[0039] Derivative link (D): Predict the temperature change trend, such as the temperature rise of a certain area is too fast, the power output can be reduced in advance to suppress overshoot and thermal shock crack, and the overshoot amount is ≤1.5℃.

[0040] Thermocouple high-density layout, i.e. ≤150mm spacing design: Can form a grid monitoring point, combined with partition independent adjustment, to ensure the uniformity of glass plate temperature, i.e. ΔT≤5℃; Thus, it can avoid defects of local stress concentration.

[0041] ‌2. Quenching kinetics optimization principle Asymmetric air nozzle array design: Upstream zone, parameters: Φ3mm hole / 15mm spacing / 30° inclination, its mechanical effect is: >120m / s high-speed airflow impact on glass surface, so as to form a high surface compressive stress layer of 90MPa; Its thermodynamic effect is: rapid cooling of the surface layer under the condition of cooling rate ≥100℃ / s, locking the surface compression lattice.

[0042] Downstream zone, parameters: Φ5mm hole / 20mm interval / 45°inclination, its mechanical effect: increase airflow coverage area, promote deep cooling, thus, form 50MPa internal tensile stress layer; its thermodynamic effect: delay core cooling, make cooling rate≤30℃ / s, realize stress gradient transition, namely, attenuation slope≤15MPa / mm.

[0043] Inclination synergistic effect: upstream 30°inclination produces tangential airflow, peels off boundary layer hot air, enhances heat exchange efficiency; downstream 45°inclination expands airflow penetration depth, balances core and surface cooling rate difference.

[0044] Stress distribution verification principle: SCALP-05 stress meter detection (≥9 points / m²), adopts 635nm polarized laser scanning, quantifies stress value through birefringence effect, controls its accuracy to be ±1MPa; high-density detection points capture stress mutation area, such as edge stress concentration, ensure that surface compressive stress≥90MPa and core tensile stress≤50MPa.

[0045] Thus, the disclosed tempered process parameter optimization system makes glass surface-core stress gradient smoothly transition, rather than mutation, can avoid self-explosion caused by uneven cooling while improving impact resistance to 1200J, so that stress imbalance rate can be less than 70%.

[0046] Further, in the foregoing step S3, for the interlayer composite key technology, a pre-humidity treatment curve can be used in PVB film treatment to realize segmented control: 0-4h: 25%RH±2%, 4-12h: 30%RH±1%, 12-24h: 28%RH±1%.

[0047] Laminating positioning system: machine vision assisted alignment, CCD resolution 0.01mm / pixel, repeated positioning accuracy ±0.05mm.

[0048] Rolling parameter matrix is shown in the following table 1: Table 1: Rolling parameter matrix

[0049] The core principle of the rolling parameter matrix is: ‌1. Temperature regulation material rheology: temperature rise reduces material yield strength, enhances plastic flowability, such as lithium battery coating treated at 120→140℃, compaction density from 3.14→3.25g / cm³. Temperature control accuracy is ±1~2℃, which can ensure transverse temperature uniformity and avoid edge and center density difference, because, when temperature difference is ±3℃, thickness deviation expands to ±0.8μm.

[0050] ‌2. Pressure-thickness synergistic mechanism: Thin material (6-8mm): low pressure (0.6MPa) matched with high speed (3.0m / min) - low pressure prevents overpressure brittle fracture, and high speed compensates for insufficient energy density caused by low pressure.

[0051] Thick material (12-19mm): high pressure (0.8MPa) combined with low speed (2.0m / min) - prolongs the action time of high pressure and promotes core densification (cake thickness ≈ 0.02 × roll diameter).

[0052] 3. Dynamic balance of speed-energy input: Speed is negatively correlated with pressure: high pressure requires reduced speed to maintain effective compaction time, such as in the 8-12mm thickness group, where a 14% increase in pressure results in a 17% decrease in speed.

[0053] Speed exceeding the limit, such as >1.75m / s, will cause poor engagement and increased wear, so it is limited to 2.0-3.0m / min, i.e. about 0.03-0.05m / s, to enhance stability.

[0054] Therefore, the execution method of the aforementioned step S3 is as follows 1. Precise temperature field control: electromagnetic heating roller with surface hardness HRC≥65 and roll face temperature difference ≤±1℃. Real-time monitoring: thermocouple grid layout with control interval ≤150mm, PID dynamic adjustment of partition power.

[0055] 2. Self-adaptive pressure loading: waist drum-shaped roller design with coaxiality ≤0.02mm to compensate for deformation under pressure and ensure uniform pressure distribution. The hydraulic system sets pressure threshold values according to thickness groups, and automatically releases pressure protection when overloaded.

[0056] 3. Speed optimization in stages: based on the formula Throughput Q = 3600 × B × s × υ × γ, the speed is calculated as follows: B roll width, s cake thickness, υ linear speed, γ cake bulk density.

[0057] Example: for the 12-19mm group, υ = 2.0m / min is selected to prevent insufficient core compaction caused by excessively high speed.

[0058] 4. Thickness grouping logic: Thin material (6-8mm): high temperature and fast pressure (120℃ / 3.0m / min) - rapid densification of the surface layer to prevent roller sticking.

[0059] Thick material (12-19mm): low temperature and slow pressure (140℃ / 2.0m / min) - deep thermal energy penetration reduces the rebound rate.

[0060] Therefore, for the aforementioned roll pressure parameter verification and boundaries, the following applies: Uniformity of thickness: under ±1℃ temperature control, thickness deviation ≤±0.5μm; deteriorate to ±1.0μm under ±3℃.

[0061] Safety boundary: pressure >0.8MPa or speed <1.5m / min easy to cause vibration, need to start the dynamic calibration of roll gap.

[0062] Therefore, it can be seen that the aforementioned roll pressure parameter matrix realizes the gradient compaction of materials from the surface to the core through thermal-mechanical-velocity coupling control, and takes into account efficiency and structural integrity.

[0063] Further, in the aforementioned step S4, the autoclave curing is improved, and temperature-pressure coupling control is used: The following is a technical analysis of the autoclave curing improvement scheme, focusing on the principles and implementation methods of temperature-pressure coupling control and crystal phase control in the cooling stage: 1. Temperature-pressure coupling control Improvement scheme: dynamic equation d𝑃 / d𝑇=0.0085𝑇−0.22 is used, where T: ℃, P: MPa; real-time pressure adjustment is realized to achieve nonlinear change of pressure with temperature during heating / cooling process.

[0064] Control principle: material rheological property matching: when 𝑇<25.9℃T<25.9℃, calculate: 0.0085𝑇−0.22<0, d𝑃 / d𝑇<0; need to reduce pressure in low temperature section to avoid internal stress cracks caused by high resin viscosity, such as significant brittleness of epoxy resin at low temperature.

[0065] When 𝑇>25.9℃, d𝑃 / d𝑇>0, high temperature section needs to increase pressure, and use material softening characteristics, i.e. viscosity decreases; thus, enhance compaction efficiency, such as 37% improvement in PVDF flowability at 140℃.

[0066] Gradient control example: when the temperature interval is 20℃→50℃, the pressure decreases from 10MPa to 8.5MPa to protect the structural integrity of low-temperature brittle materials; when the temperature interval is 100℃→150℃, the pressure increases from 5.8MPa to 8.3MPa to promote resin flow to fill micro-pores.

[0067] Execution method: adjust heating power and hydraulic valve synchronously through PID controller to track target curve with ±1℃ accuracy; pressure sensor (range 0-20MPa) and thermocouple (accuracy ±0.5℃) form closed-loop feedback to correct deviation in real time.

[0068] 2. Crystal phase control in cooling stage Improvement: Set 1-hour isothermal platform at 80℃ to inhibit the crystallization rate mutation of PVB, i.e. polyvinyl butyral. The principle is: crystallization kinetics regulation: PVB has a glass transition critical region near 80℃, and rapid cooling can trigger non-equilibrium crystallization to form spherulites with size difference > 15μm, resulting in a decrease in light transmittance or interface delamination.

[0069] Isothermal platform effect: constant temperature at the critical temperature for 1 hour to allow the ordered rearrangement of molecular chains to achieve a near-equilibrium crystalline state, at which the standard deviation of spherulite size distribution is ≤ 3μm, improving the optical uniformity of the material.

[0070] Thermodynamic mechanism: The isothermal process releases latent heat, and the enthalpy of PVB crystallization is about 110J / g, so a jacketed circulating cooling liquid such as ethylene glycol solution is needed to maintain constant temperature with a temperature fluctuation ≤ ±2℃; extending the crystal nucleus growth time can avoid the formation of microcracks caused by rapid cooling, and the crack density of the sample without isothermal treatment increases by 47%.

[0071] Integrated benefits: This scheme optimizes the solidification quality through thermal-mechanical synergistic control: temperature-pressure coupling reduces internal porosity, and the measured porosity is reduced from 0.8% to 0.2%; the isothermal crystallization platform improves the light transmittance of PVB to ≥ 91%, which is 5% higher than that of the traditional cooling process.

[0072] For the aforementioned step S5, the online detection system: infrared thermal imager with an accuracy of 0.5℃ to monitor temperature uniformity; laser diffraction instrument to detect interlayer bubbles in real time, so that the detected interlayer bubbles Φ ≤ 0.3mm. Destructive testing: shot test: impact energy is loaded in stages, i.e. from 300J→500J→700J; UV aging test: 0.55W / m²@340nm cumulative irradiation for 2000 hours.

[0073] In summary, the production process of the tempered laminated glass of the present application strictly selects the original sheet, combines the three-zone gradient tempering process, i.e. 680-700℃ temperature zone control and 8-12kPa gradient air pressure quenching, and then uses PVB interlayer precision compounding, i.e. combines 23℃ / 30%RH pre-equilibrium, 0.5mm vacuum positioning and 120-140℃ roll pressing initial pressure, and finally combines high-pressure kettle staged solidification, i.e. 1.2MPa / 135℃ holding for 120 minutes and ≤ 15℃ / h gradient cooling, so that the prepared tempered glass product has high optical performance, i.e. distortion ≤ 0.1mm / mm, strong impact resistance, i.e. 1m steel ball drop without penetration, and excellent weather resistance, i.e. no delamination in 85℃ / 85%RH / 500h environment, realizing precise control of the whole process from material to finished product. Therefore, the production process of the tempered laminated glass of the present application solves the technical problem of how to improve the production efficiency of tempered laminated glass.

[0074] The technical features of the above-described embodiments can be combined in any manner. For the sake of brevity, not all possible combinations of the technical features in the above-described embodiments are described, however, as long as the combinations of the technical features do not result in contradictions, they shall be considered as falling within the scope of the present disclosure.

[0075] The above-described embodiments only express several implementation manners of the present application, and the description is relatively specific and detailed, but it shall not be understood as a limitation on the scope of the patent right of the present application. It shall be pointed out that, for those skilled in the art, several modifications and improvements can be made without departing from the concept of the present application, and these shall fall within the protection scope of the present application. Therefore, the protection scope of the patent right of the present application shall be subject to the appended claims.

Claims

1. A production process for tempered laminated glass, characterized in that: It includes the following steps: S1: Raw glass selection and pretreatment: Float glass or ultra-clear glass is selected as the substrate, and the iron content of ultra-clear glass is controlled to be no more than 0.015%, and the light transmittance of float glass is controlled to be no less than 91.5%. The thickness of the substrate is then grouped and managed, and the deviation of substrates in the same batch is controlled to be no more than 0.1mm. Next, the substrate is cleaned using a combination of deionized water and ultrasonic cleaning to remove particles on the substrate surface, and the diameter of the residue on the substrate surface is controlled to be no more than 5μm. Finally, the substrate is laser cut and edge-grinded according to the preset size. S2: Tempering treatment: The temperature during the heating phase is controlled at 650-700°C, and the control range during the heating phase is divided into three zones for independent temperature control, namely: preheating zone 680°C ± 5°C, soaking zone 700°C ± 3°C, and equilibrium zone 690°C ± 5°C. During the quenching process, the wind pressure is controlled according to a gradient, such as: 0-3 seconds, 8kPa; 3-6 seconds, 12kPa; after 6 seconds, it is reduced to 5kPa. During stress testing, the surface compressive stress of the product is controlled to be ≥ 90MPa, and the stress layer depth is ≥ 0.1t, where t is the thickness of the glass. S3: Sandwich lamination process: During the pre-treatment of the PVB film, the temperature is controlled at 23±2°C and the humidity is 30±5% for 24 hours. During the lamination and positioning process, a vacuum suction cup fixture is used to ensure a positioning accuracy within 0.5mm. The initial pressure is exhausted and the roller pressing temperature is controlled at 120-140°C, the pressure at 0.6-0.8MPa, and the speed at 2-3m / min. S4: Autoclave curing: During the heating stage, the temperature is raised to 135±5°C at a pressure of 1.0-1.2MPa at a rate of 8-10°C / min; during the heat and pressure holding stage, the temperature is maintained for 120 minutes to ensure that the refractive index of the PVB and the glass are fully matched; during the cooling stage, the temperature is gradually reduced to below 50°C at a cooling rate of ≤15°C / h before the autoclave is opened; S5: After the tempered laminated glass is produced, the quality of the glass is monitored according to the preset quality inspection standards.

2. The process for producing tempered laminated glass according to claim 1, wherein: In step S1, when laser cutting the substrate, a CO2 laser cutting machine with a wavelength of 10.6 μm is used for cutting; the cut taper of the substrate is controlled at 0.02 mm / m, and the relationship between cutting speed and power is controlled by the following formula 1: Formula 1: P = 0.8 × e 0.05v Where, v is the cutting speed, in mm / s; P is the power, in kW.

3. The process for producing tempered laminated glass according to claim 1, wherein: In step S1, when laser cutting the substrate, a CO2 laser cutting machine with a wavelength of 10.6 μm is used for cutting; the cut taper of the substrate is controlled at 0.02 mm / m, and the relationship between the cutting speed and the power is controlled by the following formula: Formula 2: Formula 2: P = 0.8 × e 0.05v +0.02ΔT; Where v is the cutting speed in mm / s; P is the power in kW; ΔT is the change in ambient temperature in °C.

4. The process for producing tempered laminated glass according to claim 1, wherein: In step S1, after the laser cutting of the substrate is completed, the edge grinding process used is: 45° chamfering plus arc transition composite processing, and then, three-level diamond grinding wheels with specifications of 400#, 800# and 1500# are used for step-by-step polishing.

5. The process for producing tempered laminated glass according to claim 1, wherein: In step S2, the tempering process parameters are optimized as follows: Temperature field control: a PID three-closed-loop temperature control system is used to adjust the heating elements independently in different zones, and the thermocouple spacing is ≤150 mm.

6. The process for producing tempered laminated glass according to claim 1, wherein: In step S2, the tempering process parameters are optimized as follows: quenching dynamics: the nozzle array is designed as follows: upstream area: Φ3mm holes, 15mm spacing, 30° inclination, downstream area: Φ5mm holes, 20mm spacing, 45° inclination.

7. The process for producing tempered laminated glass according to claim 1, wherein: In step S2, the tempering process parameters are optimized as follows: Stress test: using a SCALP-05 stress meter, with a detection point density of ≥9 points / m².

8. The process for producing tempered laminated glass according to claim 1, wherein: In step S3, a pre-humidity treatment curve is used in the PVB film treatment to achieve segmented control: 0-4h: 25%RH±2%, 4-12h: 30%RH±1%, 12-24h: 28%RH±1%.

9. The process for producing tempered laminated glass according to claim 1, wherein: In step S3, the parameters of the assembly positioning system are: machine vision-assisted alignment, CCD resolution 0.01 mm / pixel, and repeatability accuracy ±0.05 mm.

Citation Information

Patent Citations

  • A method for manufacturing double-tempered laminated glass

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