WO2015100565A1 - 一种化学强化盐浴添加剂及其制备方法 - Google Patents

一种化学强化盐浴添加剂及其制备方法 Download PDF

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WO2015100565A1
WO2015100565A1 PCT/CN2013/090972 CN2013090972W WO2015100565A1 WO 2015100565 A1 WO2015100565 A1 WO 2015100565A1 CN 2013090972 W CN2013090972 W CN 2013090972W WO 2015100565 A1 WO2015100565 A1 WO 2015100565A1
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salt bath
additive
chemically strengthened
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glass
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PCT/CN2013/090972
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周鹏
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周鹏
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C21/00—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface
    • C03C21/001—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface in liquid phase, e.g. molten salts, solutions
    • C03C21/002—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface in liquid phase, e.g. molten salts, solutions to perform ion-exchange between alkali ions

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  • the invention relates to the field of chemical strengthening, in particular to a chemical strengthening salt bath additive and a preparation method thereof.
  • Glass materials are increasingly used in the field of electronics. Their superior surface hardness and structural strength are typical characteristics of glass materials.
  • the design of electronic terminals tends to be larger and thinner. For this reason, high-strength ultra-thin alkali glass It is widely used.
  • the biggest characteristic of this kind of glass is that the initial strength is not enough.
  • the automobile industry is also a similar situation. In order to save energy, traditional cars and electric vehicles began to use thinner glass and chemically strengthened as windows.
  • the number of effective ions in the salt bath will gradually decrease, and the number of ineffective interfering ions will increase.
  • the potassium ion concentration is lower than 10,000 ppm, the strength of the strengthened glass will not meet the requirements for use. It is necessary to replace the salt bath of the chemical strengthening method. Since the salt bath material will solidify below 350 ° C, it can only be replaced at a high temperature of more than 350 ° C. This replacement condition is relatively dangerous.
  • the replacement of the new salt bath has to go through: removing the old salt bath material at high temperature, cleaning the salt bath furnace, putting in new salt bath materials, remelting the new salt bath material, clarifying the new salt bath material, generally completing a process needs 5- 7 days, the frequency of replacement is once a month. For this reason, the production efficiency is greatly reduced.
  • salt bath materials used in the ion exchange chemical strengthening salt bath are expensive. Every time you completely replace and put in new salt bath materials, the cost is very high.
  • the technical problem to be solved by the present invention is to provide a chemically strengthened salt bath additive and a preparation method thereof for restoring the activity of a glass ion exchange chemical strengthening salt bath, improving production efficiency, and reducing production cost.
  • the technical solution adopted by the present invention is to provide a chemically strengthened salt bath additive comprising a potassium ion compound.
  • the invention also provides a preparation method of a chemically strengthened salt bath additive, comprising the steps of: weighing 5 to 70 wt% of potassium ion compound, 20-50 wt% of SiO 2 , 0-5 wt% of ZrO 2 , 0-5 wt% CaO, 0-30 wt% H 3 BO 3 , 0-30 wt% B 2 O 3 , 0-5 wt% MgO, 0-5 wt% Sb 2 O 3 0-5 wt% ZnO, 0-5 wt% TiO 2 , 0-5 wt% Al 2 O 3 mixed, heated to 1100-1500 ° C, stirred to a molten state, slowly cooled, cast or drawn Molding, annealing at a temperature of 550-650 ° C can obtain a glass chemically strengthened salt bath additive.
  • the invention has the beneficial effects that the additive is added to the spent ion exchange chemical strengthening salt bath to provide the effective ions required for the salt bath, and takes away the ions of the ineffective interference in the original failed salt bath, and recovers.
  • the salt bath activity continues to strengthen the glass with high strength.
  • the invention solves the problem that the new salt bath material must be replaced after the salt bath fails in the prior art, avoids the dangerous operation of replacing the salt bath process, ensures the production safety, avoids the production cycle delay caused by the replacement of the salt bath, and improves Production efficiency; at the same time, it also avoids the investment of new salt bath materials and reduces production costs.
  • Figure 1 is a graph showing the results of performance tests after chemical ion exchange strengthening of glass in different salt baths.
  • Embodiments of the present invention provide a glass chemically strengthened salt bath additive, the composition of which comprises a glass chemically strengthened salt bath additive, characterized in that the additive comprises a potassium ion compound.
  • weight ratio of the potassium ion compound is preferably 5 to 70 %. Further, if not particularly limited, in the following description, “%” means weight percentage "wt%”.
  • the potassium ion compound is a mixture of one or more of any potassium ion-containing compound selected from the group consisting of K 2 O, KCl, K 2 CO 3 , K 3 PO 4 , KNO 3 , K 2 at least one of SiO 3 , KOH, K 2 SO 4 , K 2 BO 4 , K 2 HPO 4 , K 3 HPO 4 , KHCO 3 , KBr, KF, KSbH 6 O 6 , KClO 4 ; preferably K 2 O At least one of KCl, K 2 CO 3 , K 3 PO 4 , KNO 3 , and K 2 SiO 3 .
  • the additive further includes SiO 2 .
  • the additive further includes at least one of ZrO 2 , CaO, H 3 BO 3 , B 2 O 3 , MgO, Sb 2 O 3 , ZnO, TiO 2 , and Al 2 O 3 .
  • the components of the additive include: 5 to 70 wt% of a potassium ion compound, 20 to 50 wt% of SiO 2 , 0 to 5 wt% of ZrO 2 , 0 to 5 wt% of CaO, and 0 to 30 wt%.
  • H 3 BO 3 0-30 wt% B 2 O 3 , 0-5 wt% MgO, 0-5 wt% Sb 2 O 3 , 0-5 wt% ZnO, 0-5 wt% TiO 2 , 0-5 Wt% of Al 2 O 3 .
  • the components of the additive include: 10 wt% K 2 O, 10 wt% KCl, 10 wt% K 2 CO 3 , 10 wt% K 3 PO 4 , 10 wt% KNO 3 , 10 Wt% K 2 SiO 3 , 20 wt% SiO 2 , 1 wt% ZrO 2 , 1 wt% CaO, 8 wt% H 3 BO 3 , 5 wt% B 2 O 3 , 1 wt% MgO, 1 wt% Sb 2 O 3 , 1 wt% ZnO, 1 wt% TiO 2 , 1 wt% Al 2 O 3 .
  • the embodiment of the invention further provides a method for preparing a glass chemically strengthened salt bath additive, comprising the steps of: weighing 5 to 70 wt% of potassium ion compound, 20-50 wt% of SiO 2 , 0-5 wt % ZrO 2 , 0-5 wt% CaO, 0-30 wt% H 3 BO 3 , 0-30 wt% B 2 O 3 , 0-5 wt% MgO, 0-5 wt% Sb 2 O 3 , 0-5 wt% ZnO, 0-5 wt% TiO 2 , 0-5 wt% Al 2 O 3 mixed, heated to 1100-1500 ° C, stirred to a molten state, slowly cooled, cast or pulled It is made into a mold and annealed at a temperature of 550-650 ° C to obtain a glass chemically strengthened salt bath additive.
  • the additive of the present invention can effectively restore the salt bath activity, which will be further described below in conjunction with specific data.
  • Test method testing the concentration changes of the interfering ions Na ions in the new and old salt baths and the additive-optimized salt bath as the main detection index, and simultaneously detecting the surface compressive stress and compressive stress depth of the glass after ion exchange, and the ions The exchanged glass was tested for three-point bending strength.
  • Test glass Corning 2318 aluminosilicate glass (100*50*0.7mm);
  • Na ion concentration measuring instrument Z-8000 atomic absorption spectrophotometer
  • Glass strength measuring instrument Instron three-point bending measuring instrument
  • Old salt bath activity recovery process conditions In the old salt bath, add 5% of the salt bath weight ratio additive, fully react with the old salt bath 400 o C, 2 hours, take out the additive, measure the ion concentration, put it into the glass Ion exchange and measure and test the glass.
  • test results are shown in Figure 1, in which the new salt bath component is nominally 99.5% industrial grade KNO 3 ; the old salt bath is the salt bath 1 has been used for 1 month after the old salt bath; the 3rd salt bath is salt Bath 2 used the additive prepared in Example 1 of the present invention to restore the active salt bath.
  • test results show that as the ion exchange progresses, the ineffective interfering ions (Na ions) in the salt bath are more and more, the concentration is significantly increased from 600 ppm to 14000 ppm, and the enhanced glass performance is degraded; the prepared old salt bath additive sufficient to react at 400 o C 2 hours, remove the additive, measured after the salt bath and optimization Na ion concentration decreased, the test glass to produce ion-exchanged glass surface after the chemical strengthening salt bath optimization Large compressive stress increases the strength of the glass.
  • Na ions interfering ions

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
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  • Organic Chemistry (AREA)
  • Glass Compositions (AREA)

Abstract

一种化学强化盐浴添加剂及其制备方法。该添加剂包括钾离子化合物，所述钾离子化合物包括K2O、KCl、K2CO3、K3PO4、KNO3、K2SiO3中的至少一种；该添加剂还包括SiO2；还包括ZrO2、CaO、H3BO3、B2O3、MgO、Sb2O3、ZnO、TiO、Al2O3中的至少一种。该添加剂加入到失效的离子交换化学强化盐浴中，可提供盐浴所需的有效离子，并带走原有失效盐浴中的无效干扰离子，重新恢复盐浴活性，继续强化出具有高强度的玻璃。

Description

一种化学强化盐浴添加剂及其制备方法 技术领域
本发明涉及化学强化领域，尤其涉及一种化学强化盐浴添加剂及其制备方法。
背景技术
玻璃材料越来越多地应用于电子领域，其优越的表面硬度以及结构强度是玻璃材料的典型特征，电子终端的设计越来越趋向于大尺寸和薄型化，为此高强度超薄碱玻璃被大量应用。这种玻璃最大的特点就是初始强度不够，必须要采用离子交换化学强化法在盐浴环境中进行离子交换增韧来增加强度。在进行离子交换时，需要在400℃左右进行2-10小时的K-Na离子交换，通过大离子对小离子的置换，在玻璃表面产生较大的压应力，从而增加玻璃强度。汽车行业也是类似的情况，为了节省能源，传统汽车和电动汽车开始采用较薄的玻璃、化学强化后作为车窗使用。
首先，随着离子交换的进行，盐浴中的有效离子数量将逐渐减少，无效干扰离子越来越多，当钾离子浓度低于10000ppm时，强化出来的玻璃强度将不能达到使用要求，为此就要更换化学强化法的盐浴，由于盐浴材料在350℃以下将会凝固，因此只能在大于350℃的高温条件下更换，这种更换条件是比较危险的。
其次，更换新的盐浴要历经：在高温下清除旧盐浴材料、清洗盐浴炉、投入新盐浴材料、重新融化新盐浴材料、澄清新盐浴材料，一般完成一个过程需要5-7天，更换的频率为一个月一次。为此，造成生产效率大幅降低。
再有，离子交换化学强化法盐浴所使用的盐浴材料，价格不菲。每次完全更换并投入新盐浴材料，成本非常高。
 技术问题
本发明所要解决的技术问题在于提供一种化学强化盐浴添加剂及其制备方法，以恢复玻璃离子交换化学强化盐浴的活性，提高生产效率，降低生产成本。
技术解决方案
本发明所采用的技术方案是提供一种化学强化盐浴添加剂，所述添加剂包括钾离子化合物。
本发明还提供一种化学强化盐浴添加剂的制备方法，包括以下步骤：称取重量百分比为5-70 wt%的钾离子化合物，20-50 wt%的SiO2, 0-5 wt%的ZrO2，0-5 wt%的CaO，0-30 wt%的H3BO3，0-30 wt%的B2O3，0-5 wt%的MgO，0-5 wt%的Sb2O3，0-5 wt%的ZnO，0-5 wt%的TiO2，0-5 wt%的Al2O3混合后加热到1100-1500℃，搅拌至熔融状态，徐冷后浇注成型或拉制成型，在550-650℃的温度下退火即可得到玻璃化学强化盐浴添加剂。
 有益效果
本发明的有益效果在于：所述添加剂加入到失效的离子交换化学强化法盐浴中，可提供盐浴所需要的有效离子，并带走原有失效盐浴中的无效干扰的离子，重新恢复盐浴活性，继续强化出的具有高强度的玻璃。本发明解决了现有技术中盐浴失效后必须更换新盐浴材料的问题，避免了更换盐浴过程的危险操作，保障了生产安全；避免了更换盐浴带来的的生产周期耽搁，提高了生产效率；同时，也避免了投入新盐浴材料，降低了生产成本。
附图说明
图1是玻璃在不同盐浴中进行化学离子交换强化后性能测试结果图。
本发明的实施方式
为了使本发明所要解决的技术问题、技术方案及有益效果更加清楚明白，以下结合附图及实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。
本发明实施例提供一种玻璃化学强化盐浴添加剂，其组分包括一种玻璃化学强化盐浴添加剂，其特征在于，所述添加剂包括钾离子化合物。
其中，所述钾离子化合物的重量比优选为5~70 %。另外，如没有特别限制，在以下说明中，“%”意思即为重量百分比“wt%”。
进一步地，所述钾离子化合物为任意含钾离子化合物的一种或几种的混合，所述钾离子化合物选自K2O、KCl、K2CO3、K3PO4、KNO3、K2SiO3、KOH、K2SO4、K2BO4、K2HPO4、K3HPO4、KHCO3、KBr、KF、KSbH6O6、KClO4中的至少一种；优选K2O、KCl、K2CO3、K3PO4、KNO3、K2SiO3中的至少一种。
进一步地，所述添加剂还包括SiO2。
进一步地，所述添加剂还包括ZrO2、CaO、H3BO3、B2O3、MgO、Sb2O3、ZnO、TiO2、Al2O3中的至少一种。
进一步地，所述添加剂的组分包括：5-70 wt%的钾离子化合物，20-50 wt%的SiO2, 0-5wt%的ZrO2，0-5wt%的CaO，0-30wt%的H3BO3，0-30wt%的B2O3，0-5wt%的MgO，0-5wt%的Sb2O3，0-5wt%的ZnO，0-5wt%的TiO2，0-5 wt%的Al2O3。
进一步地，所述添加剂的组分包括：10wt%的K2O，10 wt%的KCl，10 wt%的K2CO3，10 wt%的K3PO4，10 wt%的KNO3，10 wt%的K2SiO3，20 wt%的SiO2，1wt%的ZrO2，1wt%的CaO，8wt%的H3BO3，5wt%的B2O3，1wt%的MgO，1wt%的Sb2O3，1wt%的ZnO，1wt%的TiO2，1wt%的Al2O3。
本发明实施例还提供一种玻璃化学强化盐浴添加剂的制备方法，包括以下步骤：称取重量百分比为5-70 wt%的钾离子化合物，20-50 wt%的SiO2, 0-5 wt%的ZrO2，0-5 wt%的CaO，0-30wt%的H3BO3，0-30wt%的B2O3，0-5 wt%的MgO，0-5 wt%的Sb2O3，0-5 wt%的ZnO，0-5 wt%的TiO2，0-5 wt%的Al2O3混合后加热到1100-1500℃，搅拌至熔融状态，徐冷后浇注成型或拉制成型，在550-650℃的温度下退火即可得到玻璃化学强化盐浴添加剂。
本发明所述添加剂可有效恢复盐浴活性，以下结合具体数据进一步说明。
实施例1
称量20 wt%的KNO3, 40 wt%的K2SiO3，20 wt%的SiO2,5wt%的H3BO3，5wt%的B2O3，5wt%的Sb2O3，5wt%的Al2O3。混合均匀后放入坩埚中加热到1400-1500℃，充分搅拌至均匀，徐冷后浇注成型，在600-650℃的温度下退火即可得到玻璃化学强化盐浴添加剂。
实施例2
称量10wt%的K2O, 20 wt%的KCl、20 wt%的K3PO4、10 wt%的K2SiO3，15wt%的SiO2,7wt%的ZrO2，2wt%的CaO，8wt%的H3BO3，2wt%的MgO，3wt%的ZnO，3wt%的TiO2。混合均匀后放入坩埚中加热到1100-1200℃，充分搅拌至均匀，徐冷后拉制成2.0mm厚板状，在550-600℃的温度下退火即可得到玻璃化学强化盐浴添加剂。
试验例添加剂效果测试
试验方法：测试新、旧盐浴以及加入添加剂优化后的盐浴中的干扰离子Na离子的浓度变化作为主要检测指标，同时检测玻璃在离子交换后的表面压应力和压应力深度，并对离子交换后的玻璃做三点弯曲强度测试。
测试玻璃：康宁 2318铝硅玻璃（100*50*0.7mm）；
玻璃离子交换条件：420℃，7小时；
Na离子浓度测量仪：Z-8000原子吸收分光光度计；
玻璃表面应力和应力深度测量仪：FSM6000表面应力仪；
玻璃强度测量仪：Instron三点弯曲测量仪；
添加剂：本发明实施例1中所制备的玻璃化学强化盐浴添加剂。
旧盐浴活性恢复工艺条件:在旧盐浴中放入盐浴重量比5%的添加剂，使其与旧盐浴充分反应400oC，2小时，取出添加剂，测量离子浓度，放入玻璃进行离子交换，并对玻璃做测量、测试。
测试结果如图1所示，其中，新盐浴组分为标称99.5%工业级KNO3；旧盐浴为盐浴1已使用1个月时间后的旧盐浴；3号盐浴为盐浴2使用本发明实施例1中所制备添加剂恢复活性后的盐浴。测试结果表明，随着离子交换的进行，盐浴中无效干扰离子（Na离子）越来越多，浓度由600 ppm显著上升至14000 ppm，强化出来的玻璃性能下降；取本发明实施例1中所制备添加剂与旧盐浴在400oC下充分反应2小时，取出添加剂，测得优化后盐浴中Na离子浓度明显下降，测试玻璃在该优化盐浴中进行离子交换化学强化后玻璃表面产生较大的压应力，玻璃强度增加。

Claims (8)

  1. 一种化学强化盐浴添加剂，其特征在于，所述添加剂包括钾离子化合物。
  2. 根据权利要求1所述的化学强化盐浴添加剂，其特征在于，所述钾离子化合物的重量比为5~70 wt%。
  3. 根据权利要求1或2所述的化学强化盐浴添加剂，其特征在于，所述钾离子化合物选自K2O、KCl、K2CO3、K3PO4、KNO3、K2SiO3中的至少一种。
  4. 根据权利要求1所述的化学强化盐浴添加剂，其特征在于，所述添加剂还包括SiO2。
  5. 根据权利要求4所述的化学强化盐浴添加剂，其特征在于，所述添加剂还包括ZrO2、CaO、H3BO3、B2O3、MgO、Sb2O3、ZnO、TiO2、Al2O3中的至少一种。
  6. 根据权利要求1所述的化学强化盐浴添加剂，其特征在于：所述添加剂的组分包括：5-70 wt%的钾离子化合物，20-50 wt%的SiO2, 0-5 wt%的ZrO2，0-5wt%的CaO，0-30wt%的H3BO3，0-30wt%的B2O3，0-5wt%的MgO，0-5wt%的Sb2O3，0-5wt%的ZnO，0-5wt%的TiO2，0-5 wt%的Al2O3。
  7. 根据权利要求6所述的化学强化盐浴添加剂，其特征在于：所述添加剂原料的组分包括：10 wt%的K2O，10 wt%的KCl，10 wt%的K2CO3，10 wt%的K3PO4，10 wt%的KNO3，10 wt%的K2SiO3，20 wt%的SiO2，1wt%的ZrO2，1wt%的CaO，8 wt%的H3BO3，5 wt%的B2O3，1 wt%的MgO，1 wt%的Sb2O3，1 wt%的ZnO，1 wt%的TiO2，1 wt%的Al2O3。
  8. 一种化学强化盐浴添加剂的制备方法，包括以下步骤：称取重量百分比为5-70 wt%的钾离子化合物，20-50 wt%的SiO2, 0-5 wt%的ZrO2，0-5 wt%的CaO，0-30 wt%的H3BO3，0-30 wt%的B2O3，0-5 wt%的MgO，0-5 wt%的Sb2O3，0-5 wt%的ZnO，0-5 wt%的TiO2，0-5 wt%的Al2O3混合后加热到1100-1500℃，搅拌至熔融状态，徐冷后浇注成型或拉制成型，在550-650℃的温度下退火即可得到玻璃化学强化盐浴添加剂。
PCT/CN2013/090972 2013-12-30 2013-12-30 一种化学强化盐浴添加剂及其制备方法 WO2015100565A1 (zh)

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CN111217735A (zh) * 2018-11-27 2020-06-02 上海汇伦医药科技有限公司 赛洛多辛中间体的制备方法
CN113845315A (zh) * 2021-10-21 2021-12-28 成都光明光电股份有限公司 离子交换盐浴添加剂
CN115304289A (zh) * 2022-08-26 2022-11-08 成都光明光电股份有限公司 适用于含银盐浴的盐浴添加剂
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CN111217735A (zh) * 2018-11-27 2020-06-02 上海汇伦医药科技有限公司 赛洛多辛中间体的制备方法
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CN113845315A (zh) * 2021-10-21 2021-12-28 成都光明光电股份有限公司 离子交换盐浴添加剂
CN115304289A (zh) * 2022-08-26 2022-11-08 成都光明光电股份有限公司 适用于含银盐浴的盐浴添加剂
CN115304289B (zh) * 2022-08-26 2023-07-04 成都光明光电股份有限公司 适用于含银盐浴的盐浴添加剂

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