CN104098274B - A kind of glass enamel and preparation method thereof for leadless environment-friendly easy cut ampule - Google Patents
A kind of glass enamel and preparation method thereof for leadless environment-friendly easy cut ampule Download PDFInfo
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- 239000011521 glass Substances 0.000 title claims abstract description 198
- 239000003708 ampul Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 210000003298 dental enamel Anatomy 0.000 title abstract 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 74
- 239000003795 chemical substances by application Substances 0.000 claims description 50
- 239000000843 powder Substances 0.000 claims description 42
- 239000002002 slurry Substances 0.000 claims description 38
- 239000011787 zinc oxide Substances 0.000 claims description 37
- 239000000463 material Substances 0.000 claims description 32
- 238000009837 dry grinding Methods 0.000 claims description 30
- 241001391944 Commicarpus scandens Species 0.000 claims description 29
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 28
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 28
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 23
- 239000011734 sodium Substances 0.000 claims description 22
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 22
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 21
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 20
- 238000002844 melting Methods 0.000 claims description 18
- 230000008018 melting Effects 0.000 claims description 18
- 229910021538 borax Inorganic materials 0.000 claims description 17
- 239000004328 sodium tetraborate Substances 0.000 claims description 17
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 15
- 239000006004 Quartz sand Substances 0.000 claims description 14
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 14
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 14
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 14
- 239000006060 molten glass Substances 0.000 claims description 13
- 238000010791 quenching Methods 0.000 claims description 13
- 230000000171 quenching effect Effects 0.000 claims description 13
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 10
- 239000004408 titanium dioxide Substances 0.000 claims description 10
- 230000007613 environmental effect Effects 0.000 claims description 8
- 239000003995 emulsifying agent Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 238000001238 wet grinding Methods 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 229910052593 corundum Inorganic materials 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 3
- 238000010304 firing Methods 0.000 abstract description 33
- 239000003605 opacifier Substances 0.000 abstract description 13
- 239000000758 substrate Substances 0.000 description 22
- 238000000498 ball milling Methods 0.000 description 12
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 description 11
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 description 11
- 229940116411 terpineol Drugs 0.000 description 11
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 229910011255 B2O3 Inorganic materials 0.000 description 2
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Inorganic materials [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
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Abstract
Description
技术领域technical field
本发明属于玻璃釉合成技术领域，具体涉及一种无铅环保易折安瓿用玻璃色釉及其制备方法。The invention belongs to the technical field of glass glaze synthesis, and in particular relates to a lead-free, environment-friendly and easy-to-break glass colored glaze for ampoule and a preparation method thereof.
背景技术Background technique
国外在20世纪60年代已广泛在曲颈安瓿的颈槽内涂上与玻璃本身线膨胀系数有差异的色釉，经退火后产生预应力的色环易折安瓿或点刻痕易折安瓿。易折安瓿使用方便，折断时极少产生玻屑，不污染药液，有利于保障人体健康，我国在20世纪80年代逐渐推广应用。In foreign countries in the 1960s, the neck groove of the curved neck ampoule was widely coated with a color glaze that is different from the linear expansion coefficient of the glass itself. After annealing, a prestressed color ring or a point-marked easy-to-break ampoule was produced. The easy-to-break ampoule is easy to use, rarely produces glass debris when broken, does not pollute the liquid medicine, and is conducive to protecting human health. It was gradually popularized and used in my country in the 1980s.
早期易折安瓿色釉采用的是有铅易溶色釉，基本能够满足易折安瓿的需要。随着现代科技的发展以及科学发展观的贯彻，有铅易溶色釉已不能满足人们对生态和健康的需求，研发无毒、环保的无铅易溶色釉已成为当前最重要的课题之一。但是，同时实现易折安瓿釉的无铅化和满足膨胀系数、釉烧温度、白度的要求，一直是易折安瓿瓶研究的瓶颈。所以，在对曲颈安瓿易折机理分析的基础上，如何采用更优质的釉料，使其能够达到无毒、白度良好、釉烧温度和膨胀系数适宜、成本低是亟待解决的技术问题。The early breakable ampoule color glazes used lead-soluble color glazes, which can basically meet the needs of breakable ampoules. With the development of modern science and technology and the implementation of the scientific concept of development, lead-soluble colored glazes can no longer meet people's needs for ecology and health. The research and development of non-toxic and environmentally friendly lead-free soluble colored glazes has become one of the most important issues at present. one. However, realizing the lead-free glaze of the easy-break ampoule and meeting the requirements of expansion coefficient, glaze firing temperature, and whiteness at the same time has always been the bottleneck of the research on the break-away ampoule. Therefore, on the basis of the analysis of the easy-breaking mechanism of the curved neck ampoule, how to use a higher-quality glaze to achieve non-toxicity, good whiteness, suitable glaze firing temperature and expansion coefficient, and low cost is a technical problem that needs to be solved urgently. .
发明内容Contents of the invention
本发明的目的在于提供一种无铅环保易折安瓿用玻璃色釉及其制备方法，制得的釉料无毒，白度良好，成本低并且膨胀系数、釉烧温度适宜。The object of the present invention is to provide a lead-free, environmentally friendly and easy-to-break glass colored glaze for ampoules and a preparation method thereof. The prepared glaze is non-toxic, has good whiteness, low cost, and suitable expansion coefficient and glaze firing temperature.
为实现上述目的，本发明采用如下的技术方案：To achieve the above object, the present invention adopts the following technical solutions:
一种无铅环保易折安瓿用玻璃色釉，包括基釉和乳浊剂，其中基釉的组分按重量份数计，包括30～50份的SiO2，10～25份的Na2O，10～25份的B2O3，13～18份的CaO，5～10份的ZnO，1～5份的BaO，0.5～2份的Al2O3，0～10份的TiO2和0～5份的SnO2；所述乳浊剂为基釉的质量的2～12％。A lead-free, environmentally friendly and easy-to-break glass glaze for ampoules, including a base glaze and an opacifying agent, wherein the components of the base glaze include 30-50 parts of SiO 2 and 10-25 parts of Na 2 O in parts by weight. , 10-25 parts of B 2 O 3 , 13-18 parts of CaO, 5-10 parts of ZnO, 1-5 parts of BaO, 0.5-2 parts of Al 2 O 3 , 0-10 parts of TiO 2 and 0-5 parts of SnO 2 ; the opacifying agent is 2-12% of the mass of the base glaze.
一种无铅环保易折安瓿用玻璃色釉，包括基釉和乳浊剂，其中基釉的组分按重量份数计，包括32～48份的SiO2，15～25份的Na2O，12～22份的B2O3，13～18份的CaO，5～10份的ZnO，1～5份的BaO，0.5～2份的Al2O3，0～10份的TiO2和0～5份的SnO2；所述乳浊剂为基釉的质量的2～12％。A lead-free, environmentally friendly and easy-to-break glass glaze for ampoules, including a base glaze and an opacifying agent, wherein the components of the base glaze include 32-48 parts of SiO 2 and 15-25 parts of Na 2 O in parts by weight , 12-22 parts of B 2 O 3 , 13-18 parts of CaO, 5-10 parts of ZnO, 1-5 parts of BaO, 0.5-2 parts of Al 2 O 3 , 0-10 parts of TiO 2 and 0-5 parts of SnO 2 ; the opacifying agent is 2-12% of the mass of the base glaze.
一种无铅环保安瓿用玻璃色釉的制备方法，包括以下步骤：A preparation method of glass colored glaze for lead-free environmental protection ampoules, comprising the following steps:
(1)按照基釉组分的重量份数计，将30～50份SiO2，10～25份Na2O，10～25份B2O3，13～18份CaO，5～10份ZnO，1～5份BaO，0.5～2份Al2O3，0～10份TiO2，0～5份SnO2混合均匀，得到配合料；(1) According to the parts by weight of the base glaze components, 30-50 parts of SiO 2 , 10-25 parts of Na 2 O, 10-25 parts of B 2 O 3 , 13-18 parts of CaO, 5-10 parts of ZnO , 1-5 parts of BaO, 0.5-2 parts of Al 2 O 3 , 0-10 parts of TiO 2 , and 0-5 parts of SnO 2 are uniformly mixed to obtain batch materials;
(2)将配合料进行熔制，使配合料完全熔融，得到玻璃液；(2) Melting the batch material to completely melt the batch material to obtain molten glass;
(3)将玻璃液进行水淬得到玻璃熔块；(3) Carry out water quenching to glass liquid to obtain glass frit;
(4)将玻璃熔块进行湿磨，得到玻璃浆；(4) wet grinding the glass frit to obtain glass slurry;
(5)将玻璃浆过250目筛后在烘箱里烘干，得到玻璃粉，将玻璃粉再放入快速球磨罐进行干磨，干磨后得到的粉体即为基釉；(5) Dry the glass slurry in an oven after passing through a 250-mesh sieve to obtain glass powder, then put the glass powder into a quick ball mill jar for dry grinding, and the powder obtained after dry grinding is the base glaze;
(6)将基釉与经过预处理的外加乳浊剂在混料设备中混合均匀，得到无铅环保易折安瓿用玻璃色釉；其中，乳浊剂的加入量为基釉质量的2～12％。(6) Mix the base glaze with the pretreated external opacifying agent in the mixing equipment to obtain the glass color glaze for lead-free environmental protection easy-folding ampoules; wherein, the addition of the opacifying agent is 2-2% of the quality of the base glaze 12%.
所述乳浊剂为TiO2。The opacifying agent is TiO 2 .
所述SiO2来自石英砂，Na2O来自碳酸钠或硼砂，B2O3来自硼砂，CaO来自碳酸钙，ZnO来自氧化锌，BaO来自碳酸钡，Al2O3来自氢氧化铝，TiO2来自二氧化钛，SnO2来自二氧化锡。The SiO2 comes from quartz sand, Na2O comes from sodium carbonate or borax, B2O3 comes from borax, CaO comes from calcium carbonate, ZnO comes from zinc oxide , BaO comes from barium carbonate, Al2O3 comes from aluminum hydroxide , TiO2 from titanium dioxide and SnO2 from tin dioxide.
所述熔制的温度为1200-1340℃。The melting temperature is 1200-1340°C.
所述熔制是在电阻炉中进行的。The melting is carried out in a resistance furnace.
所述外加乳浊剂的预处理具体为：将乳浊剂的粒径研磨至小于250目。The pretreatment of adding the emulsifying agent is specifically: grinding the particle size of the emulsifying agent to less than 250 mesh.
所述湿磨是在快速球磨罐中进行的，并且球磨时间为30-40min；干磨是在快速球磨罐中进行的，并且干磨的时间为15-20min。The wet milling is carried out in a quick ball milling jar, and the ball milling time is 30-40 minutes; the dry milling is carried out in a fast ball milling jar, and the dry milling time is 15-20 minutes.
与现有技术相比，本发明具有的有益效果：本发明在基釉玻璃粉中加入预处理后的2～12％乳浊剂，在混料设备中进行粉磨混合，使其充分混合均匀，粒度达到250目以上，涂在安瓿玻璃上能够达到易折安瓿要求的白度、烧成温度、膨胀系数。在熔制的时候加入TiO2或SnO2以提高折射率和光泽度，本发明的玻璃色釉包括基釉和乳浊剂，并且基釉组分包括SiO2、Na2O、B2O3、CaO、ZnO、BaO、Al2O3、TiO2和SnO2，基釉体系化学稳定性良好、不易潮解，外加乳浊剂后是一种无铅环保型玻璃乳白色釉，并且白度能够达到75％以上、釉烧温度适宜、膨胀系数适宜、成本低、适于我国现阶段大量采用的低硼硅系统安瓿，并且最终的釉烧温度范围在580～660℃之间，符合要求。本发明的玻璃色釉与安瓿瓶的膨胀系数有合理差异，玻璃色釉的膨胀系数在(85～110)×10-7/℃范围内，可满足易折安瓿玻璃乳白色釉的使用要求。在曲颈安瓿颈部表面涂一层极薄的玻璃色釉，由于玻璃色釉与安瓿瓶之间存在膨胀系数的差异，便会在安瓿颈部的凹处形成集中的应力，使安瓿易于折断。这一特性使得玻璃安瓿既便于使用，又安全卫生，完全可以取代实际生产中有毒的铅质釉。本发明也可用于制备彩釉玻璃。Compared with the prior art, the present invention has beneficial effects: the present invention adds pretreated 2-12% opacifier to the base glaze glass powder, and grinds and mixes it in a mixing device to make it fully mixed and uniform , the particle size can reach more than 250 mesh, and the whiteness, firing temperature, and expansion coefficient required by the easy-folding ampoule can be achieved when coated on the ampoule glass. Add TiO 2 or SnO 2 when melting to increase the refractive index and gloss. The glass color glaze of the present invention includes base glaze and opacifying agent, and the base glaze components include SiO 2 , Na 2 O, B 2 O 3 , CaO, ZnO, BaO, Al 2 O 3 , TiO 2 and SnO 2 , the base glaze system has good chemical stability and is not easy to deliquescence. After adding an opacifying agent, it is a lead-free and environmentally friendly glass milky white glaze, and the whiteness can reach Above 75%, the glaze firing temperature is suitable, the expansion coefficient is suitable, the cost is low, and it is suitable for the low borosilicate system ampoules widely used in China at this stage, and the final glaze firing temperature range is between 580 and 660°C, which meets the requirements. The expansion coefficient of the glass colored glaze of the present invention is reasonably different from that of the ampoule bottle, and the expansion coefficient of the glass colored glaze is in the range of (85-110)×10 -7 /°C, which can meet the use requirements of the easy-folding ampoule glass milky white glaze. Apply a very thin layer of glass colored glaze on the neck surface of the curved neck ampoule. Due to the difference in expansion coefficient between the glass colored glaze and the ampoule bottle, concentrated stress will be formed in the concave part of the ampoule neck, making the ampoule easy to break. . This feature makes the glass ampoule easy to use, safe and hygienic, and can completely replace the toxic lead glaze in actual production. The invention can also be used for preparing colored glaze glass.
附图说明Description of drawings
图1为本发明的技术路线图。Fig. 1 is a technical roadmap of the present invention.
具体实施方式detailed description
一种无铅环保易折安瓿用玻璃色釉的制备方法，包括基釉和乳浊剂，所述基釉的组分按重量份数计，包括30～50份SiO2，10～25份Na2O，10～25份B2O3，13～18份CaO，5～10份ZnO，1～5份BaO，0.5～2份Al2O3，0～10份TiO2和0～5份SnO2；基釉中SiO2、Na2O、B2O3、CaO、ZnO、BaO、Al2O3的质量份数的和为100份；所述玻璃色釉还包括外加乳浊剂TiO2，乳浊剂占基釉质量的2～12％。A method for preparing a lead-free, environmentally friendly and easy-to-break glass colored glaze for ampoules, comprising a base glaze and an opacifying agent. The components of the base glaze include 30-50 parts of SiO 2 , 10-25 parts of Na 2 O, 10-25 parts of B 2 O 3 , 13-18 parts of CaO, 5-10 parts of ZnO, 1-5 parts of BaO, 0.5-2 parts of Al 2 O 3 , 0-10 parts of TiO 2 and 0-5 parts SnO 2 ; the sum of the mass parts of SiO 2 , Na 2 O, B 2 O 3 , CaO, ZnO, BaO, and Al 2 O 3 in the base glaze is 100 parts; the glass color glaze also includes an additional opacifying agent TiO 2. The opacifying agent accounts for 2-12% of the mass of the base glaze.
上述无铅环保易折安瓿用玻璃色釉的制备方法，包括以下步骤：The preparation method of the above-mentioned lead-free environment-friendly easy-folding ampoule glass colored glaze comprises the following steps:
(1)按照基釉组分的重量份数，将30～50份SiO2，10～25份Na2O，10～25份B2O3，13～18份CaO，5～10份ZnO，1～5份BaO，0.5～2份Al2O3，0～10份TiO2，0～5份SnO2在混料设备中混合均匀，得到配合料；其中，SiO2来自石英砂，Na2O来自碳酸钠或硼砂，B2O3来自硼砂，CaO来自碳酸钙，ZnO来自氧化锌，BaO来自碳酸钡，Al2O3来自氢氧化铝，TiO2来自二氧化钛，SnO2来自二氧化锡。具体操作为：通过计算，按照基釉中各组分的质量份数，将石英砂、碳酸钠、硼砂、碳酸钙、氧化锌、碳酸钡、氢氧化铝、二氧化钛、二氧化锡等原料混合均匀，得到配合料。(1) According to the parts by weight of the base glaze components, 30-50 parts of SiO 2 , 10-25 parts of Na 2 O, 10-25 parts of B 2 O 3 , 13-18 parts of CaO, 5-10 parts of ZnO, 1-5 parts of BaO, 0.5-2 parts of Al 2 O 3 , 0-10 parts of TiO 2 , and 0-5 parts of SnO 2 are uniformly mixed in the mixing equipment to obtain batch materials; among them, SiO 2 comes from quartz sand, Na 2 O is from sodium carbonate or borax, B2O3 is from borax, CaO is from calcium carbonate, ZnO is from zinc oxide , BaO is from barium carbonate, Al2O3 is from aluminum hydroxide, TiO2 is from titanium dioxide , and SnO2 is from tin dioxide. The specific operation is: through calculation, mix quartz sand, sodium carbonate, borax, calcium carbonate, zinc oxide, barium carbonate, aluminum hydroxide, titanium dioxide, tin dioxide and other raw materials evenly according to the mass fraction of each component in the base glaze , to get the batch material.
(2)将配合料在电阻炉中于1200-1340℃下进行熔制，使配合料完全熔融，得到玻璃液；(2) Melting the batch material in a resistance furnace at 1200-1340°C to completely melt the batch material to obtain molten glass;
(3)将玻璃液进行水淬得到玻璃熔块；(3) Carry out water quenching to glass liquid to obtain glass frit;
(4)将玻璃熔块放入到快速球磨罐中，并加入一定量的水和球进行快速球磨30-40min，得到玻璃浆；(4) Put the glass frit into the quick ball milling jar, and add a certain amount of water and balls to carry out the quick ball milling for 30-40min to obtain the glass slurry;
(5)将玻璃浆过250目筛后在烘箱里烘干，得到玻璃粉，将玻璃粉再放入快速球磨罐进行干磨15-20min，干磨后得到的粉体即为基釉；(5) Pass the glass slurry through a 250-mesh sieve and dry it in an oven to obtain glass powder, then put the glass powder into a quick ball mill jar for dry grinding for 15-20 minutes, and the powder obtained after dry grinding is the base glaze;
(6)将基釉与粒径小于250目的外加乳浊剂在混料设备中混合均匀，得到无铅环保易折安瓿用玻璃色釉；其中，乳浊剂的加入量为基釉质量的2～12％。(6) Mix the base glaze and the extra opacifying agent with a particle size less than 250 meshes in the mixing equipment to obtain the glass color glaze for lead-free environmental protection and easy to break ampoules; wherein, the addition of the opacifying agent is 2% of the mass of the base glaze ~12%.
本发明制备的玻璃色釉的使用方法，具体包括以下步骤：The using method of the glass color glaze prepared by the present invention specifically comprises the following steps:
(1)在制备的色釉玻璃粉中添加松油醇制备成釉浆：(1) Add terpineol to the prepared colored glaze glass powder to prepare glaze slurry:
(2)通过刮板将步骤(1)所得到的釉浆在安瓿玻璃基体上进行施釉，之后进行干燥；(2) Glaze the glaze slurry obtained in step (1) on the ampoule glass substrate by a scraper, and then dry it;
(3)将干燥后的带釉玻璃基体送入釉烧炉烧成，即可。其中，烧成温度为580～660℃，(3) Send the dried glazed glass substrate into a glaze firing furnace for firing. Among them, the firing temperature is 580-660°C,
下面结合实施例对本发明作进一步的详细说明。Below in conjunction with embodiment the present invention is described in further detail.
实施例1Example 1
一种无铅环保易折安瓿用玻璃色釉，包括基釉和乳浊剂，其中基釉的组分按重量份数计，包括48份的SiO2，15份的Na2O，12份的B2O3，15份的CaO，6份的ZnO，3份的BaO，1份的Al2O3和2份的SnO2；所述乳浊剂为基釉的质量的2％。A kind of lead-free environment-friendly glass colored glaze for easy breaking ampoules, including base glaze and opacifying agent, wherein the components of the base glaze are calculated in parts by weight, including 48 parts of SiO 2 , 15 parts of Na 2 O, 12 parts of B 2 O 3 , 15 parts of CaO, 6 parts of ZnO, 3 parts of BaO, 1 part of Al 2 O 3 and 2 parts of SnO 2 ; the opacifier is 2% of the mass of the base glaze.
上述无铅环保易折安瓿用玻璃色釉的制备方法，包括以下步骤：The preparation method of the above-mentioned lead-free environment-friendly easy-folding ampoule glass colored glaze comprises the following steps:
(1)按照基釉的组分，将石英砂、碳酸钠、硼砂、碳酸钙、氧化锌、碳酸钡、氢氧化铝和二氧化锡在混合设备中混合均匀，得到配合料；(1) According to the components of the base glaze, quartz sand, sodium carbonate, borax, calcium carbonate, zinc oxide, barium carbonate, aluminum hydroxide and tin dioxide are uniformly mixed in a mixing device to obtain batch materials;
(2)将配合料在电阻炉中于1340℃下进行熔制，使配合料完全熔融，得到玻璃液；(2) Melting the batch material in a resistance furnace at 1340°C to completely melt the batch material to obtain molten glass;
(3)将玻璃液进行水淬得到玻璃熔块；(3) Carry out water quenching to glass liquid to obtain glass frit;
(4)将玻璃熔块放入到快速球磨罐中，并加入一定量的水和球进行快速球磨40min，得到玻璃浆；(4) Put the glass frit into the quick ball mill jar, and add a certain amount of water and balls for quick ball milling for 40 minutes to obtain glass slurry;
(5)将玻璃浆过250目筛后在烘箱里烘干，得到玻璃粉，将玻璃粉再放入快速球磨罐进行干磨15min，干磨后得到的粉体即为基釉；(5) Pass the glass slurry through a 250-mesh sieve and dry it in an oven to obtain glass powder, then put the glass powder into a quick ball mill jar for dry grinding for 15 minutes, and the powder obtained after dry grinding is the base glaze;
(6)将基釉与粒径小于250目的外加乳浊剂在混料机中混合均匀，得到无铅环保易折安瓿用玻璃色釉；其中，乳浊剂的加入量为基釉质量的2％。(6) Mix the base glaze and the extra opacifying agent with a particle size less than 250 meshes in a mixer to obtain a lead-free, environmentally friendly and easy-to-break glass colored glaze for ampoules; wherein, the addition of the opacifying agent is 2% of the quality of the base glaze %.
使用时，将制备的玻璃色釉与松油醇进行混合，得到釉浆，通过刮板在安瓿玻璃基体上进行施釉，之后进行干燥；将干燥后带釉的玻璃基体送入釉烧炉在660℃下烧成。When in use, the prepared glass colored glaze is mixed with terpineol to obtain a glaze slurry, which is glazed on the ampoule glass substrate by a scraper, and then dried; the dried glazed glass substrate is sent into a glaze firing furnace at 660 Firing at ℃.
实施例2Example 2
一种无铅环保易折安瓿用玻璃色釉，包括基釉和乳浊剂，其中基釉的组分按重量份数计，包括42份的SiO2，21份的Na2O，12份的B2O3，15份的CaO，6份的ZnO，3份的BaO，1份的Al2O3和4份的SnO2；所述乳浊剂为基釉的质量的4％。A lead-free, environmentally friendly and easy-to-break glass glaze for ampoules, including a base glaze and an opacifying agent, wherein the components of the base glaze are calculated in parts by weight, including 42 parts of SiO 2 , 21 parts of Na 2 O, 12 parts of B 2 O 3 , 15 parts of CaO, 6 parts of ZnO, 3 parts of BaO, 1 part of Al 2 O 3 and 4 parts of SnO 2 ; the opacifier is 4% of the mass of the base glaze.
上述无铅环保易折安瓿用玻璃色釉的制备方法，包括以下步骤：The preparation method of the above-mentioned lead-free environment-friendly easy-folding ampoule glass colored glaze comprises the following steps:
(1)按照基釉的组分，将石英砂、碳酸钠、硼砂、碳酸钙、氧化锌、碳酸钡、氢氧化铝和二氧化锡在混合设备中混合均匀，得到配合料；(1) According to the components of the base glaze, quartz sand, sodium carbonate, borax, calcium carbonate, zinc oxide, barium carbonate, aluminum hydroxide and tin dioxide are uniformly mixed in a mixing device to obtain batch materials;
(2)将配合料在电阻炉中于1300℃下进行熔制，使配合料完全熔融，得到玻璃液；(2) Melt the batch material in a resistance furnace at 1300°C to completely melt the batch material to obtain molten glass;
(3)将玻璃液进行水淬得到玻璃熔块；(3) Carry out water quenching to glass liquid to obtain glass frit;
(4)将玻璃熔块放入到快速球磨罐中，并加入一定量的水和球进行快速球磨40min，得到玻璃浆；(4) Put the glass frit into the quick ball mill jar, and add a certain amount of water and balls for quick ball milling for 40 minutes to obtain glass slurry;
(5)将玻璃浆过250目筛后在烘箱里烘干，得到玻璃粉，将玻璃粉再放入球磨罐进行干磨15min，干磨后得到的粉体即为基釉；(5) Pass the glass slurry through a 250-mesh sieve and dry it in an oven to obtain glass powder, then put the glass powder into a ball mill jar for dry grinding for 15 minutes, and the powder obtained after dry grinding is the base glaze;
(6)将基釉与粒径小于250目的外加乳浊剂在混料机中混合均匀，得到无铅环保易折安瓿用玻璃色釉；其中，乳浊剂的加入量为基釉质量的4％。(6) Mix the base glaze and the extra emulsifying agent less than 250 meshes in particle size in the mixer to obtain lead-free environmental friendly easy-fold glass colored glaze for ampoule; wherein, the adding amount of the emulsifying agent is 4% of the mass of the base glaze %.
使用时，将制备的玻璃色釉与松油醇进行混合，得到釉浆，通过刮板在安瓿玻璃基体上进行施釉，之后进行干燥；将干燥后带釉的玻璃基体送入釉烧炉在640℃下烧成。When in use, the prepared glass colored glaze is mixed with terpineol to obtain a glaze slurry, which is glazed on the ampoule glass substrate by a scraper, and then dried; the dried glazed glass substrate is sent into a glaze firing furnace at 640 Firing at ℃.
实施例3Example 3
一种无铅环保易折安瓿用玻璃色釉，包括基釉和乳浊剂，其中基釉的组分按重量份数计，包括42份的SiO2，15份的Na2O，16份的B2O3，15份的CaO，8份的ZnO，3份的BaO，1份的Al2O3和4份的TiO2；所述乳浊剂为基釉的质量的6％。A kind of glass color glaze for lead-free environment-friendly and easy to break ampoules, comprises base glaze and opacifying agent, wherein the components of base glaze include 42 parts of SiO 2 , 15 parts of Na 2 O, 16 parts of B 2 O 3 , 15 parts of CaO, 8 parts of ZnO, 3 parts of BaO, 1 part of Al 2 O 3 and 4 parts of TiO 2 ; the opacifier is 6% of the mass of the base glaze.
上述无铅环保易折安瓿用玻璃色釉的制备方法，包括以下步骤：The preparation method of the above-mentioned lead-free environment-friendly easy-folding ampoule glass colored glaze comprises the following steps:
(1)按照基釉的组分，将石英砂、碳酸钠、硼砂、碳酸钙、氧化锌、碳酸钡、氢氧化铝和二氧化钛在混合设备中混合均匀，得到配合料；(1) According to the components of the base glaze, quartz sand, sodium carbonate, borax, calcium carbonate, zinc oxide, barium carbonate, aluminum hydroxide and titanium dioxide are uniformly mixed in a mixing device to obtain a batch;
(2)将配合料在电阻炉中于1320℃下进行熔制，使配合料完全熔融，得到玻璃液；(2) Melt the batch material in a resistance furnace at 1320°C to completely melt the batch material to obtain molten glass;
(3)将玻璃液进行水淬得到玻璃熔块；(3) Carry out water quenching to glass liquid to obtain glass frit;
(4)将玻璃熔块放入到快速球磨罐中，并加入一定量的水和球进行快速球磨40min，得到玻璃浆；(4) Put the glass frit into the quick ball mill jar, and add a certain amount of water and balls for quick ball milling for 40 minutes to obtain glass slurry;
(5)将玻璃浆过250目筛后在烘箱里烘干，得到玻璃粉，将玻璃粉再放入快速球磨罐进行干磨15min，干磨后得到的粉体即为基釉；(5) Pass the glass slurry through a 250-mesh sieve and dry it in an oven to obtain glass powder, then put the glass powder into a quick ball mill jar for dry grinding for 15 minutes, and the powder obtained after dry grinding is the base glaze;
(6)将基釉与粒径小于250目的外加乳浊剂在混料机中混合均匀，得到无铅环保易折安瓿用玻璃色釉；其中，乳浊剂的加入量为基釉质量的6％。(6) The base glaze and the extra opacifying agent with a particle size less than 250 meshes are uniformly mixed in a mixer to obtain a lead-free, environmentally friendly and easy-to-break glass colored glaze for ampoules; wherein, the addition of the opacifying agent is 6% of the quality of the base glaze %.
使用时，将制备的玻璃色釉与松油醇进行混合，得到釉浆，通过刮板在安瓿玻璃基体上进行施釉，之后进行干燥；将干燥后带釉的玻璃基体送入釉烧炉在650℃下烧成。When in use, the prepared glass colored glaze is mixed with terpineol to obtain a glaze slurry, which is glazed on the ampoule glass substrate by a scraper, and then dried; the dried glazed glass substrate is sent into a glaze firing furnace at 650 Firing at ℃.
实施例4Example 4
一种无铅环保易折安瓿用玻璃色釉，包括基釉和乳浊剂，其中基釉的组分按重量份数计，包括36份的SiO2，15份的Na2O，22份的B2O3，15份的CaO，8份的ZnO，3份的BaO，1份的Al2O3和2份的TiO2；所述乳浊剂为基釉的质量的8％。A lead-free, environmentally friendly and easy-to-break glass glaze for ampoules, including a base glaze and an opacifying agent, wherein the components of the base glaze include 36 parts of SiO 2 , 15 parts of Na 2 O, 22 parts of B 2 O 3 , 15 parts of CaO, 8 parts of ZnO, 3 parts of BaO, 1 part of Al 2 O 3 and 2 parts of TiO 2 ; the opacifier is 8% of the mass of the base glaze.
上述无铅环保易折安瓿用玻璃色釉的制备方法，包括以下步骤：The preparation method of the above-mentioned lead-free environment-friendly easy-folding ampoule glass colored glaze comprises the following steps:
(1)按照基釉的组分，将石英砂、碳酸钠、硼砂、碳酸钙、氧化锌、碳酸钡、氢氧化铝和二氧化钛在混合设备中混合均匀，得到配合料；(1) According to the components of the base glaze, quartz sand, sodium carbonate, borax, calcium carbonate, zinc oxide, barium carbonate, aluminum hydroxide and titanium dioxide are uniformly mixed in a mixing device to obtain a batch;
(2)将配合料在电阻炉中于1280℃下进行熔制，使配合料完全熔融，得到玻璃液；(2) Melting the batch material in a resistance furnace at 1280°C to completely melt the batch material to obtain molten glass;
(3)将玻璃液进行水淬得到玻璃熔块；(3) Carry out water quenching to glass liquid to obtain glass frit;
(4)将玻璃熔块放入到快速球磨罐中，并加入一定量的水和球进行快速球磨40min，得到玻璃浆；(4) Put the glass frit into the quick ball mill jar, and add a certain amount of water and balls for quick ball milling for 40 minutes to obtain glass slurry;
(5)将玻璃浆过250目筛后在烘箱里烘干，得到玻璃粉，将玻璃粉再放入快速球磨罐进行干磨15min，干磨后得到的粉体即为基釉；(5) Pass the glass slurry through a 250-mesh sieve and dry it in an oven to obtain glass powder, then put the glass powder into a quick ball mill jar for dry grinding for 15 minutes, and the powder obtained after dry grinding is the base glaze;
(6)将基釉与粒径小于250目的外加乳浊剂在混料机中混合均匀，得到无铅环保易折安瓿用玻璃色釉；其中，乳浊剂的加入量为基釉质量的8％。(6) Mix the base glaze and the extra opacifying agent with a particle diameter less than 250 meshes in a mixer to obtain a lead-free, environmentally friendly and easy-to-break glass colored glaze for ampoules; wherein, the addition of the opacifying agent is 8% of the quality of the base glaze %.
使用时，将制备的玻璃色釉与松油醇进行混合，得到釉浆，通过刮板在安瓿玻璃基体上进行施釉，之后进行干燥；将干燥后带釉的玻璃基体送入釉烧炉在630℃下烧成。When in use, the prepared glass colored glaze is mixed with terpineol to obtain a glaze slurry, which is glazed on the ampoule glass substrate by a scraper, and then dried; the dried glazed glass substrate is sent into a glaze firing furnace at 630 Firing at ℃.
实施例5Example 5
一种无铅环保易折安瓿用玻璃色釉，包括基釉和乳浊剂，其中基釉的组分按重量份数计，包括36份的SiO2，15份的Na2O，22份的B2O3，15份的CaO，8份的ZnO，3份的BaO，1份的Al2O3和5份的TiO2；所述乳浊剂为基釉的质量的10％。A lead-free, environmentally friendly and easy-to-break glass glaze for ampoules, including a base glaze and an opacifying agent, wherein the components of the base glaze include 36 parts of SiO 2 , 15 parts of Na 2 O, 22 parts of B 2 O 3 , 15 parts of CaO, 8 parts of ZnO, 3 parts of BaO, 1 part of Al 2 O 3 and 5 parts of TiO 2 ; the opacifier is 10% of the mass of the base glaze.
上述无铅环保易折安瓿用玻璃色釉的制备方法，包括以下步骤：The preparation method of the above-mentioned lead-free environment-friendly easy-folding ampoule glass colored glaze comprises the following steps:
(1)按照基釉的组分，将石英砂、碳酸钠、硼砂、碳酸钙、氧化锌、碳酸钡、氢氧化铝和二氧化钛在混合设备中混合均匀，得到配合料；(1) According to the components of the base glaze, quartz sand, sodium carbonate, borax, calcium carbonate, zinc oxide, barium carbonate, aluminum hydroxide and titanium dioxide are uniformly mixed in a mixing device to obtain a batch;
(2)将配合料在电阻炉中于1280℃下进行熔制，使配合料完全熔融，得到玻璃液；(2) Melting the batch material in a resistance furnace at 1280°C to completely melt the batch material to obtain molten glass;
(3)将玻璃液进行水淬得到玻璃熔块；(3) Carry out water quenching to glass liquid to obtain glass frit;
(4)将玻璃熔块放入到球磨罐中，并加入一定量的水和球进行快速球磨40min，得到玻璃浆；(4) Put the glass frit into a ball mill jar, and add a certain amount of water and balls for rapid ball milling for 40 minutes to obtain glass slurry;
(5)将玻璃浆过250目筛后在烘箱里烘干，得到玻璃粉，将玻璃粉再放入快速球磨罐进行干磨15min，干磨后得到的粉体即为基釉；(5) Pass the glass slurry through a 250-mesh sieve and dry it in an oven to obtain glass powder, then put the glass powder into a quick ball mill jar for dry grinding for 15 minutes, and the powder obtained after dry grinding is the base glaze;
(6)将基釉与粒径小于250目的外加乳浊剂在混料机中混合均匀，得到无铅环保易折安瓿用玻璃色釉；其中，乳浊剂的加入量为基釉质量的10％。(6) Mix the base glaze and the extra opacifying agent with a particle size less than 250 meshes in a mixer to obtain lead-free, environmentally friendly and easy-to-break glass colored glaze for ampoules; wherein, the addition of the opacifying agent is 10% of the quality of the base glaze %.
使用时，将制备的玻璃色釉与松油醇进行混合，得到釉浆，通过刮板在安瓿玻璃基体上进行施釉，之后进行干燥；将干燥后带釉的玻璃基体送入釉烧炉在640℃下烧成。When in use, the prepared glass colored glaze is mixed with terpineol to obtain a glaze slurry, which is glazed on the ampoule glass substrate by a scraper, and then dried; the dried glazed glass substrate is sent into a glaze firing furnace at 640 Firing at ℃.
实施例6Example 6
一种无铅环保易折安瓿用玻璃色釉，包括基釉和乳浊剂，其中基釉的组分按重量份数计，包括36份的SiO2，15份的Na2O，22份的B2O3，15份的CaO，8份的ZnO，3份的BaO，1份的Al2O3和8份的TiO2；所述乳浊剂为基釉的质量的12％。A lead-free, environmentally friendly and easy-to-break glass glaze for ampoules, including a base glaze and an opacifying agent, wherein the components of the base glaze include 36 parts of SiO 2 , 15 parts of Na 2 O, 22 parts of B 2 O 3 , 15 parts of CaO, 8 parts of ZnO, 3 parts of BaO, 1 part of Al 2 O 3 and 8 parts of TiO 2 ; the opacifier is 12% of the mass of the base glaze.
上述无铅环保易折安瓿用玻璃色釉的制备方法，包括以下步骤：The preparation method of the above-mentioned lead-free environment-friendly easy-folding ampoule glass colored glaze comprises the following steps:
(1)按照基釉的组分，将石英砂、碳酸钠、硼砂、碳酸钙、氧化锌、碳酸钡、氢氧化铝和二氧化钛在混合设备中混合均匀，得到配合料；(1) According to the components of the base glaze, quartz sand, sodium carbonate, borax, calcium carbonate, zinc oxide, barium carbonate, aluminum hydroxide and titanium dioxide are uniformly mixed in a mixing device to obtain a batch;
(2)将配合料在电阻炉中于1280℃下进行熔制，使配合料完全熔融，得到玻璃液；(2) Melting the batch material in a resistance furnace at 1280°C to completely melt the batch material to obtain molten glass;
(3)将玻璃液进行水淬得到玻璃熔块；(3) Carry out water quenching to glass liquid to obtain glass frit;
(4)将玻璃熔块放入到快速球磨罐中，并加入一定量的水和球进行快速球磨40min，得到玻璃浆；(4) Put the glass frit into the quick ball mill jar, and add a certain amount of water and balls for quick ball milling for 40 minutes to obtain glass slurry;
(5)将玻璃浆过250目筛后在烘箱里烘干，得到玻璃粉，将玻璃粉再放入快速球磨罐进行干磨15min，干磨后得到的粉体即为基釉；(5) Pass the glass slurry through a 250-mesh sieve and dry it in an oven to obtain glass powder, then put the glass powder into a quick ball mill jar for dry grinding for 15 minutes, and the powder obtained after dry grinding is the base glaze;
(6)将基釉与粒径小于250目的外加乳浊剂在混料机中混合均匀，得到无铅环保易折安瓿用玻璃色釉；其中，乳浊剂的加入量为基釉质量的12％。(6) Mix the base glaze and the extra opacifying agent with a particle size less than 250 meshes in a mixer to obtain a lead-free, environmentally friendly and easy-to-break glass glaze for ampoules; wherein, the addition of the opacifying agent is 12% of the quality of the base glaze. %.
使用时，将制备的玻璃色釉与松油醇进行混合，得到釉浆，通过刮板在安瓿玻璃基体上进行施釉，之后进行干燥；将干燥后带釉的玻璃基体送入釉烧炉在650℃下烧成。When in use, the prepared glass colored glaze is mixed with terpineol to obtain a glaze slurry, which is glazed on the ampoule glass substrate by a scraper, and then dried; the dried glazed glass substrate is sent into a glaze firing furnace at 650 Firing at ℃.
实施例7Example 7
一种无铅环保易折安瓿用玻璃色釉，包括基釉和乳浊剂，其中基釉的组分按重量份数计，包括36份的SiO2，15份的Na2O，22份的B2O3，15份的CaO，8份的ZnO，3份的BaO，1份的Al2O3、2份的TiO2和2份的SnO2；所述乳浊剂为基釉的质量的6％。A lead-free, environmentally friendly and easy-to-break glass glaze for ampoules, including a base glaze and an opacifying agent, wherein the components of the base glaze include 36 parts of SiO 2 , 15 parts of Na 2 O, 22 parts of B 2 O 3 , 15 parts of CaO, 8 parts of ZnO, 3 parts of BaO, 1 part of Al 2 O 3 , 2 parts of TiO 2 and 2 parts of SnO 2 ; the opacifier is the mass of the base glaze 6%.
上述无铅环保易折安瓿用玻璃色釉的制备方法，包括以下步骤：The preparation method of the above-mentioned lead-free environment-friendly easy-folding ampoule glass colored glaze comprises the following steps:
(1)按照基釉的组分，将石英砂、碳酸钠、硼砂、碳酸钙、氧化锌、碳酸钡、氢氧化铝、二氧化钛和二氧化锡在混合设备中混合均匀，得到配合料；(1) According to the components of the base glaze, quartz sand, sodium carbonate, borax, calcium carbonate, zinc oxide, barium carbonate, aluminum hydroxide, titanium dioxide and tin dioxide are uniformly mixed in a mixing device to obtain a batch;
(2)将配合料在电阻炉中于1280℃下进行熔制，使配合料完全熔融，得到玻璃液；(2) Melting the batch material in a resistance furnace at 1280°C to completely melt the batch material to obtain molten glass;
(3)将玻璃液进行水淬得到玻璃熔块；(3) Carry out water quenching to glass liquid to obtain glass frit;
(4)将玻璃熔块放入到快速球磨罐中，并加入一定量的水和球进行快速球磨40min，得到玻璃浆；(4) Put the glass frit into the quick ball mill jar, and add a certain amount of water and balls for quick ball milling for 40 minutes to obtain glass slurry;
(5)将玻璃浆过250目筛后在烘箱里烘干，得到玻璃粉，将玻璃粉再放入快速球磨罐进行干磨15min，干磨后得到的粉体即为基釉；(5) Pass the glass slurry through a 250-mesh sieve and dry it in an oven to obtain glass powder, then put the glass powder into a quick ball mill jar for dry grinding for 15 minutes, and the powder obtained after dry grinding is the base glaze;
(6)将基釉与粒径小于250目的外加乳浊剂在混料机中混合均匀，得到无铅环保易折安瓿用玻璃色釉；其中，乳浊剂的加入量为基釉质量的6％。(6) The base glaze and the extra opacifying agent with a particle size less than 250 meshes are uniformly mixed in a mixer to obtain a lead-free, environmentally friendly and easy-to-break glass colored glaze for ampoules; wherein, the addition of the opacifying agent is 6% of the quality of the base glaze %.
使用时，将制备的玻璃色釉与松油醇进行混合，得到釉浆，通过刮板在安瓿玻璃基体上进行施釉，之后进行干燥；将干燥后带釉的玻璃基体送入釉烧炉在640℃下烧成。When in use, the prepared glass colored glaze is mixed with terpineol to obtain a glaze slurry, which is glazed on the ampoule glass substrate by a scraper, and then dried; the dried glazed glass substrate is sent into a glaze firing furnace at 640 Firing at ℃.
实施例8Example 8
一种无铅环保易折安瓿用玻璃色釉，包括基釉和乳浊剂，其中基釉的组分按重量份数计，包括34份的SiO2，20.5份的Na2O，21份的B2O3，18份的CaO，5份的ZnO，1份的BaO和0.5份的Al2O3；所述乳浊剂为基釉的质量的7％。A lead-free, environmentally friendly and easy-to-break glass glaze for ampoules, including a base glaze and an opacifying agent, wherein the components of the base glaze are calculated in parts by weight, including 34 parts of SiO 2 , 20.5 parts of Na 2 O, 21 parts of B 2 O 3 , 18 parts of CaO, 5 parts of ZnO, 1 part of BaO and 0.5 parts of Al 2 O 3 ; the opacifier is 7% of the mass of the base glaze.
上述无铅环保易折安瓿用玻璃色釉的制备方法，包括以下步骤：The preparation method of the above-mentioned lead-free environment-friendly easy-folding ampoule glass colored glaze comprises the following steps:
(1)按照基釉的组分，将石英砂、碳酸钠、硼砂、碳酸钙、氧化锌、碳酸钡和氢氧化铝在混合设备中混合均匀，得到配合料；(1) According to the components of the base glaze, quartz sand, sodium carbonate, borax, calcium carbonate, zinc oxide, barium carbonate and aluminum hydroxide are uniformly mixed in a mixing device to obtain a batch;
(2)将配合料在电阻炉中于1260℃下进行熔制，使配合料完全熔融，得到玻璃液；(2) Melting the batch material in a resistance furnace at 1260°C to completely melt the batch material to obtain molten glass;
(3)将玻璃液进行水淬得到玻璃熔块；(3) Carry out water quenching to glass liquid to obtain glass frit;
(4)将玻璃熔块放入到球磨罐中，并加入一定量的水和球进行快速湿磨30min，得到玻璃浆；(4) Put the glass frit into the ball mill jar, and add a certain amount of water and balls for quick wet milling for 30 minutes to obtain glass slurry;
(5)将玻璃浆过250目筛后在烘箱里烘干，得到玻璃粉，将玻璃粉再放入快速球磨罐进行干磨20min，干磨后得到的粉体即为基釉；(5) Pass the glass slurry through a 250-mesh sieve and dry it in an oven to obtain glass powder, then put the glass powder into a quick ball mill jar for dry grinding for 20 minutes, and the powder obtained after dry grinding is the base glaze;
(6)将基釉与粒径小于250目的外加乳浊剂在混料机中混合均匀，得到无铅环保易折安瓿用玻璃色釉；其中，乳浊剂的加入量为基釉质量的7％。(6) The base glaze and the extra opacifying agent with a particle size less than 250 meshes are uniformly mixed in a mixer to obtain a lead-free, environmentally friendly and easy-to-break glass colored glaze for ampoules; wherein, the addition of the opacifying agent is 7% of the quality of the base glaze %.
使用时，将制备的玻璃色釉与松油醇进行混合，得到釉浆，通过刮板在安瓿玻璃基体上进行施釉，之后进行干燥；将干燥后带釉的玻璃基体送入釉烧炉在580℃下烧成。When in use, the prepared glass colored glaze is mixed with terpineol to obtain a glaze slurry, which is glazed on the ampoule glass substrate by a scraper, and then dried; the dried glazed glass substrate is sent into a glaze firing furnace at 580 Firing at ℃.
实施例9Example 9
一种无铅环保易折安瓿用玻璃色釉，包括基釉和乳浊剂，其中基釉的组分按重量份数计，包括32份的SiO2，25份的Na2O，10份的B2O3，17份的CaO，9份的ZnO，5份的BaO，2份的Al2O3、6份的TiO2和5份的SnO2；所述乳浊剂为基釉的质量的9％。A kind of lead-free environment-friendly glass colored glaze for easy breaking ampoules, including base glaze and opacifying agent, wherein the components of the base glaze are calculated in parts by weight, including 32 parts of SiO 2 , 25 parts of Na 2 O, 10 parts of B 2 O 3 , 17 parts of CaO, 9 parts of ZnO, 5 parts of BaO, 2 parts of Al 2 O 3 , 6 parts of TiO 2 and 5 parts of SnO 2 ; the opacifier is the mass of the base glaze 9%.
上述无铅环保易折安瓿用玻璃色釉的制备方法，包括以下步骤：The preparation method of the above-mentioned lead-free environment-friendly easy-folding ampoule glass colored glaze comprises the following steps:
(1)按照基釉的组分，将石英砂，碳酸钠、硼砂、碳酸钙、氧化锌、碳酸钡、氢氧化铝、二氧化钛和二氧化锡在混合设备中混合均匀，得到配合料；(1) According to the components of the base glaze, quartz sand, sodium carbonate, borax, calcium carbonate, zinc oxide, barium carbonate, aluminum hydroxide, titanium dioxide and tin dioxide are uniformly mixed in a mixing device to obtain a batch;
(2)将配合料在电阻炉中于1200℃下进行熔制，使配合料完全熔融，得到玻璃液；(2) Melting the batch material in a resistance furnace at 1200°C to completely melt the batch material to obtain molten glass;
(3)将玻璃液进行水淬得到玻璃熔块；(3) Carry out water quenching to glass liquid to obtain glass frit;
(4)将玻璃熔块放入到快速球磨罐中，并加入一定量的水和球进行湿磨35min，得到玻璃浆；(4) Put the glass frit into a quick ball mill jar, and add a certain amount of water and balls to wet mill for 35 minutes to obtain glass slurry;
(5)将玻璃浆过250目筛后在烘箱里烘干，得到玻璃粉，将玻璃粉再放入快速球磨罐进行干磨15min，干磨后得到的粉体即为基釉；(5) Pass the glass slurry through a 250-mesh sieve and dry it in an oven to obtain glass powder, then put the glass powder into a quick ball mill jar for dry grinding for 15 minutes, and the powder obtained after dry grinding is the base glaze;
(6)将基釉与粒径小于250目的外加乳浊剂在混料机中混合均匀，得到无铅环保易折安瓿用玻璃色釉；其中，乳浊剂的加入量为基釉质量的9％。(6) The base glaze and the extra opacifying agent with a particle size less than 250 meshes are uniformly mixed in a mixer to obtain a lead-free, environmentally friendly and easy-to-break glass colored glaze for ampoules; wherein, the addition of the opacifying agent is 9% of the quality of the base glaze %.
使用时，将制备的玻璃色釉与松油醇进行混合，得到釉浆，通过刮板在安瓿玻璃基体上进行施釉，之后进行干燥；将干燥后带釉的玻璃基体送入釉烧炉在600℃下烧成。When in use, the prepared glass colored glaze is mixed with terpineol to obtain a glaze slurry, which is then glazed on the ampoule glass substrate by a scraper, and then dried; the dried glazed glass substrate is sent into a glaze firing furnace at 600 Firing at ℃.
实施例10Example 10
一种无铅环保易折安瓿用玻璃色釉，包括基釉和乳浊剂，其中基釉的组分按重量份数计，包括39份的SiO2，10份的Na2O，25份的B2O3，13份的CaO，10份的ZnO，2份的BaO和1份的Al2O3；所述乳浊剂为基釉的质量的3％。A kind of glass color glaze for lead-free environment-friendly and easy to break ampoules, comprises base glaze and opacifying agent, wherein the components of base glaze are calculated in parts by weight, including 39 parts of SiO 2 , 10 parts of Na 2 O, 25 parts of B 2 O 3 , 13 parts of CaO, 10 parts of ZnO, 2 parts of BaO and 1 part of Al 2 O 3 ; the opacifying agent is 3% of the mass of the base glaze.
上述无铅环保易折安瓿用玻璃色釉的制备方法，包括以下步骤：The preparation method of the above-mentioned lead-free environment-friendly easy-folding ampoule glass colored glaze comprises the following steps:
(1)按照基釉的组分，将石英砂、碳酸钠、硼砂、碳酸钙、氧化锌、碳酸钡和氢氧化铝在混合设备中混合均匀，得到配合料；(1) According to the components of the base glaze, quartz sand, sodium carbonate, borax, calcium carbonate, zinc oxide, barium carbonate and aluminum hydroxide are uniformly mixed in a mixing device to obtain a batch;
(2)将配合料在电阻炉中于1260℃下进行熔制，使配合料完全熔融，得到玻璃液；(2) Melting the batch material in a resistance furnace at 1260°C to completely melt the batch material to obtain molten glass;
(3)将玻璃液进行水淬得到玻璃熔块；(3) Carry out water quenching to glass liquid to obtain glass frit;
(4)将玻璃熔块放入到快速球磨罐中，并加入一定量的水和球进行湿磨35min，得到玻璃浆；(4) Put the glass frit into a quick ball mill jar, and add a certain amount of water and balls to wet mill for 35 minutes to obtain glass slurry;
(5)将玻璃浆过250目筛后在烘箱里烘干，得到玻璃粉，将玻璃粉再放入快速球磨罐进行干磨20min，干磨后得到的粉体即为基釉；(5) Pass the glass slurry through a 250-mesh sieve and dry it in an oven to obtain glass powder, then put the glass powder into a quick ball mill jar for dry grinding for 20 minutes, and the powder obtained after dry grinding is the base glaze;
(6)将基釉与粒径小于250目的外加乳浊剂在混料机中混合均匀，得到无铅环保易折安瓿用玻璃色釉；其中，乳浊剂的加入量为基釉质量的3％。(6) Mix the base glaze and the extra opacifying agent with a particle size less than 250 meshes in a mixer to obtain lead-free, environmentally friendly and easy-to-break glass colored glaze for ampoules; wherein, the addition of the opacifying agent is 3% of the quality of the base glaze %.
使用时，将制备的玻璃色釉与松油醇进行混合，得到釉浆，通过刮板在安瓿玻璃基体上进行施釉，之后进行干燥；将干燥后带釉的玻璃基体送入釉烧炉在620℃下烧成。When in use, the prepared glass colored glaze is mixed with terpineol to obtain a glaze slurry, which is glazed on the ampoule glass substrate by a scraper, and then dried; the dried glazed glass substrate is sent into a glaze firing furnace at 620 Firing at ℃.
本发明实施例1-7所制备的玻璃色釉性能对比：The performance comparison of the glass color glaze prepared by the embodiment of the present invention 1-7:
表1实施例1-7的釉烧结果The glaze firing result of table 1 embodiment 1-7
从上表可以看出，实施例5制备的玻璃色釉的白度、光泽度都很好。As can be seen from the above table, the whiteness and gloss of the glass colored glaze prepared in Example 5 are all very good.
本发明提供一种能够应用在医用安瓿上起到使安瓿易折和装饰功能的技术，在曲颈安瓿颈部表面涂一层极薄的色釉，由于色釉与安瓿瓶之间存在膨胀系数的差异，便会在安瓿颈部的凹处形成集中的应力，使安瓿易于折断。这一特性使得玻璃安瓿既便于使用，又安全卫生；也可用于制备彩釉玻璃。The invention provides a technology that can be applied to medical ampoules to make the ampoules easy to fold and decorate. A layer of extremely thin color glaze is applied to the neck surface of the curved neck ampoule, because there is an expansion coefficient between the color glaze and the ampoule bottle If the difference is small, concentrated stress will be formed in the recess of the neck of the ampoule, making the ampoule easy to break. This feature makes the glass ampoule easy to use, safe and hygienic; it can also be used to prepare colored glaze glass.
通过大量的实验研究发现若只用熔加法在基釉系统中添加基釉质量的0～5％SnO2、0～10％TiO2时，乳浊效果不明显；而通过磨加法在上述基釉玻璃粉中外加基釉质量的2％～12％TiO2时，乳浊效果良好。所以本发明采用双加法，先熔加基釉质量5％TiO2(或SnO2)在基釉中，用于提高色釉的折射率和光泽度，再磨加基釉质量的10％TiO2乳浊效果最佳，最终的釉烧温度范围在580～660℃之间，符合要求。通过白度仪对色釉白度测定，能够达到75％以上。Through a large number of experimental studies, it is found that if only 0-5% SnO 2 and 0-10% TiO 2 are added to the base glaze system by melting and adding, the opacification effect is not obvious; When 2% to 12% TiO 2 of the base glaze mass is added to the glass powder, the opacification effect is good. Therefore, the present invention adopts a double addition method, first melting and adding 5% TiO 2 (or SnO 2 ) of the base glaze in the base glaze to improve the refractive index and gloss of the color glaze, and then grinding and adding 10% TiO 2 of the base glaze The opacification effect is the best, and the final glaze firing temperature range is between 580 and 660°C, which meets the requirements. The whiteness of the glaze can be measured by a whiteness meter, and it can reach more than 75%.
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