CN114369376A - 高亮光钴黑色素及制备方法 - Google Patents
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- XUMBMVFBXHLACL-UHFFFAOYSA-N Melanin Chemical compound O=C1C(=O)C(C2=CNC3=C(C(C(=O)C4=C32)=O)C)=C2C4=CNC2=C1C XUMBMVFBXHLACL-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 17
- 239000010941 cobalt Substances 0.000 title claims abstract description 17
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 229920002545 silicone oil Polymers 0.000 claims abstract description 13
- QDOXWKRWXJOMAK-UHFFFAOYSA-N chromium(III) oxide Inorganic materials O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910015667 MoO4 Inorganic materials 0.000 claims abstract description 7
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Inorganic materials O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000011248 coating agent Substances 0.000 claims abstract description 4
- 238000000576 coating method Methods 0.000 claims abstract description 4
- 239000000047 product Substances 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000012065 filter cake Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 238000000498 ball milling Methods 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000010902 jet-milling Methods 0.000 claims description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 239000000706 filtrate Substances 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 239000000446 fuel Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000003345 natural gas Substances 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 239000002002 slurry Substances 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000001238 wet grinding Methods 0.000 claims description 2
- 229910019934 (NH4)2MoO4 Inorganic materials 0.000 claims 1
- 238000004321 preservation Methods 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 10
- 229910044991 metal oxide Inorganic materials 0.000 abstract description 9
- 238000006243 chemical reaction Methods 0.000 abstract description 8
- 229910052596 spinel Inorganic materials 0.000 abstract description 7
- 239000011029 spinel Substances 0.000 abstract description 7
- -1 ferrous metal oxide Chemical class 0.000 abstract description 6
- 239000000843 powder Substances 0.000 abstract description 6
- 150000004706 metal oxides Chemical class 0.000 abstract description 4
- XOFYZVNMUHMLCC-ZPOLXVRWSA-N prednisone Chemical compound O=C1C=C[C@]2(C)[C@H]3C(=O)C[C@](C)([C@@](CC4)(O)C(=O)CO)[C@@H]4[C@@H]3CCC2=C1 XOFYZVNMUHMLCC-ZPOLXVRWSA-N 0.000 abstract description 4
- 238000004040 coloring Methods 0.000 abstract description 3
- 238000005345 coagulation Methods 0.000 abstract description 2
- 230000015271 coagulation Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 239000013618 particulate matter Substances 0.000 abstract description 2
- 229920001296 polysiloxane Polymers 0.000 abstract description 2
- 239000000839 emulsion Substances 0.000 abstract 1
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 239000001023 inorganic pigment Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- 210000003298 dental enamel Anatomy 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- 239000000049 pigment Substances 0.000 description 3
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000549 coloured material Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/0009—Pigments for ceramics
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- 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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
- C09C3/063—Coating
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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Abstract
本发明公开一种高亮光钴黑色素及制备方法。本发明的高亮光钴黑色素配方由如下按质量份计的成分组成:Co2O312~14份,Cr2O346~49份,CuO 26~29份,ZnO 3.7~4.5份,MnO25~6份,LiF 0.5‑1份,Bi2031‑2份,K2MnO41‑2份,(NH4)2MoO41‑2份,乳化硅油0.48‑1份。本发明通过引入矿化剂对有色金属氧化物进行表面离子化包覆处理,使其均匀附着在有色金属氧化物颗粒表面,降低颗粒的电离能ΔE,促进反应完成。乳化硅油的引入能够避免细粉颗粒的假凝聚,且由于颗粒物质的电离彻底,更容易得到纯粹的尖晶石结构着色材料。
Description
技术领域
本发明属于无机颜料技术领域,具体涉及一种高亮光钴黑色素及制备方法。
背景技术
无机颜料在搪瓷釉料里加入3-5%的黑色无机颜料涂覆在制品表面烧成后的产品,普通的黑色素无机颜料会导致制品的表面颜色发生改变,如制品表面亮度差、颜色偏黄色或偏红相、着色力差等。
现有黑色无机颜料的生产配方和工艺无法形成纯粹的尖晶石晶体。尖晶石晶体可看作氧离子形成立方最紧密堆积体,再由x离子占据64个四面体空隙的1/8,即8个A位,Y离子占据32个八面体空隙的1/2,即16个B位。由此得出尖晶石单位晶胞的通式为X8Y16032,简约后常写作:XY204。现有产品的生产方法和技术原理是:将有色金属氧化物粉碎成微米级(15-80μm)粉末,经1110-1120℃煅烧合成。参与反应物质之间的化学合成需要很高的温度使参与反应的物质电离,以便克服化学反应能ΔE完成合成。但参与反应物质的电离不彻底,所以很难得到纯粹的尖晶石结构,有部分未完全反应的金属氧化物游离于晶体外,形成晶体和玻璃态的混合物。
发明内容
本发明的目的在于针对现有技术中所存在的上述快陷,提供一种高亮光钴黑色素及制备方法。
本发明的技术方案为:
一种高亮光钴黑色素,其配方由如下按质量份计的成分组成:Co2O3 12~14份,Cr2O3 46~49份,CuO26~29份,ZnO 3.7~4.5份,MnO2 5~6份,LiF 0.5-1份,Bi203 1-2份,K2MnO4 1-2份,(NH4)2MoO4 1-2份,乳化硅油0.48-1份。
上述高亮光钴黑色素的制备方法,包括如下步骤:
(1)准备如下质量份计的原材料:Co2O3 12~14份,Cr2O3 46~49份,Cu0 26~29份,ZnO3.7~4.5份,MnO2 5~6份,LiF 0.5-1份,Bi203 1-2份,生料入混合机混合均匀,控制混合均匀度≧97%,得混合生料;
(2)表面离子化包覆处理:在步骤(1)所得混合生料中,先加入水,再加入(NH4)2MoO41-2份、K2MnO4 1-2份和乳化硅油0.5-1份进行球磨,料浆经压滤机液固分离,滤液入池循环使用,湿滤饼经干燥粉碎后,气流粉碎至细度D97≤10μm,装入匣缽堆码在窑车上;
(3)窑车送入煅烧窑,点燃天然气燃料,程序升温,室温升至1110~1150℃,升温的速度控制在150-200℃/h,保温6-7小时,控制炉窑的温差小于5℃,熄火窑内自然降温至100~150℃出窑,自然冷却得熟料;
(4)冷却好的熟料送入球磨机,加水湿磨,球磨至D97≤10μm,出料入漂洗桶,加水漂洗,出料压滤,滤饼经干燥,气流粉碎,控制细度D97≤3um,即得高亮光钴黑色素。
进一步地,步骤(2)中,所加水的质量为步骤(1)所得混合生料质量的70%~90%。
上述高亮光钴黑色素引入搪瓷制品中,经过830℃左后的高温试验,所得制品表面具有像镜面一样的高亮度,带蓝黑色相。
本发明的有益效果在于:
本发明将配方中所有的有色金属氧化物进行均匀混合后球磨,然后超微处理,粒径要求D97≤10μm。同时,引入矿化剂对有色金属氧化物进行表面离子化包覆处理,使其均匀附着在有色金属氧化物颗粒表面,参与反应物质之间的化学合成反应实质上变成了颗粒物质与离子间的反应,而颗粒物质在离子物质的作用下使颗粒的电离能ΔE下降,从而降低了化学反应能ΔE完成合成。引入乳化硅油降低粉体颗粒的表面能,避免细粉颗粒的假凝聚。由于参与反应的颗粒物质的电离彻底,所以很容易得到纯粹的尖晶石结构着色材料。
本发明经过1110~1150℃高温合成,得到具有稳定、纯粹的尖晶石结构的混合晶体着色材料。本发明高亮光钴黑色素引入搪瓷制品中,其产品经过830℃左后的高温试验,其制品表面具有像镜面一样的高亮度,带蓝黑色相。
具体实施方式
下面结合具体实施例对本发明作进一步详细的描述。
本发明中使用的设备为常观设备,比如气流粉碎设备、粉体表面离子化处理设备、压滤设备、煅烧炉窑等。
实施例1
高亮光钴黑色素的制备方法,包括如下步骤:
(1)先按Co2O3 14KG,Cr2O3 49KG,CuO 26KG,ZnO 4.5KG,MnO 5KG,Bi203 1KG,LiF0.5KG配置原料,然后均匀混合,控制均匀度≥97%;
(2)在步骤(1)所得混合物中加入80KG(混合物重的80%)的水,再加入乳化硅油0.48KG、K2MnO4 1KG和(NH4)2MoO4 1.5KG(三者共同作为分散剂),在球磨机中球磨,然后烘干,气流粉碎;
(3)将粉体装入圆形的耐高温的匣钵内放入旋转焰的炉窑内煅烧,从室温开始升温至1120℃,升温的速度控制在180℃/h左右,保温7小时,控制炉窑的温度为1120±5℃,最后自然冷却到室温;
(4)将烧成的颜料放入球磨机中球磨、烘干后,气流粉碎至D97≤3μm,即得产品。
实施例2
本实施例与实施例1的制备过程基本相同,不同之处在于:
(a)Co2O3 12KG,Cr2O3 48KG,CuO 28KG,ZnO 3.7KG,MnO 6KG,Bi203 1.5KG,LiF0.8KG;
(b)水的加入量为70KG(混合物重的70%);
(c)分散剂组成:乳化硅油0.6KG、K2MnO4 1.5KG和(NH4)2MoO4 1KG。
实施例3
本实施例与实施例1的制备过程基本相同,不同之处在于:
(a)Co2O3 12KG,Cr2O3 46KG,CuO 29KG,ZnO 4KG,MnO 6KG,Bi203 2KG,LiF 1KG;
(b)水的加入量为90KG(混合物重的90%);
(c)分散剂组成:乳化硅油1KG、K2MnO4 2KG和(NH4)2MoO4 2KG。
经过830℃左后的高温试验,上述实施例所得产品均具有纯粹的尖晶石结构,从而产品能够赋予两个重要特性,即高温中的稳定以及能够在高温的状态下经得起釉料的溶解。
采用本发明生产的高亮光钴黑色素引入到搪瓷制品中,所得制品具有高亮度带蓝黑色相的稳定性能。
Claims (6)
1.一种高亮光钴黑色素,其特征在于,其配方由如下按质量份计的成分组成:Co2O3 12~14份,Cr2O3 46~49份,CuO 26~29份,ZnO 3.7~4.5份,MnO2 5~6份,LiF 0.5-1份,Bi2031-2份,K2MnO4 1-2份,(NH4)2MoO4 1-2份,乳化硅油0.48-1份。
2.如权利要求1所述的高亮光钴黑色素的制备方法,其特征在于,包括如下步骤:
(1)准备如下质量份计的原材料:Co2O3 12~14份,Cr2O3 46~49份,CuO26~29份,ZnO3.7~4.5份,MnO2 5~6份,LiF 0.5-1份,Bi203 1-2份,生料入混合机混合均匀,得混合生料;
(2)表面离子化包覆处理:在步骤(1)所得混合生料中,先加入水,再加入(NH4)2MoO41-2份、K2MnO4 1-2份和乳化硅油0.5-1份进行球磨,料浆经压滤机液固分离,滤液入池循环使用,湿滤饼经干燥粉碎后,气流粉碎至细度D97≤10μm,装入匣缽堆码在窑车上;
(3)窑车送入煅烧窑,点燃天然气燃料,程序升温,室温升至1110~1150℃,保温6-7小时,控制炉窑的温差小于5℃,熄火窑内自然降温至100~150℃出窑,自然冷却得熟料;
(4)冷却好的熟料送入球磨机,加水湿磨,球磨至D97≤10μm,出料入漂洗桶,加水漂洗,出料压滤,滤饼经干燥,气流粉碎,控制细度D97≤3um,即得高亮光钴黑色素。
3.如权利要求2所述的高亮光钴黑色素的制备方法,其特征在于,步骤(1)中,控制混合均匀度≧97%。
4.如权利要求2所述的高亮光钴黑色素的制备方法,其特征在于,步骤(2)中,所加水的质量为步骤(1)所得混合生料质量的70%~90%。
5.如权利要求2所述的高亮光钴黑色素的制备方法,其特征在于,步骤(3)中,升温的速度控制在150-200℃/h。
6.如权利要求1所述的高亮光钴黑色素在搪瓷制品中的应用。
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Citations (12)
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