CN109608906B - 一种超细氧化铝包裹型钼钒酸铋黄色颜料及其制备方法 - Google Patents
一种超细氧化铝包裹型钼钒酸铋黄色颜料及其制备方法 Download PDFInfo
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- CN109608906B CN109608906B CN201910064978.7A CN201910064978A CN109608906B CN 109608906 B CN109608906 B CN 109608906B CN 201910064978 A CN201910064978 A CN 201910064978A CN 109608906 B CN109608906 B CN 109608906B
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- 239000001052 yellow pigment Substances 0.000 title claims abstract description 76
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 title claims abstract description 29
- DKUYEPUUXLQPPX-UHFFFAOYSA-N dibismuth;molybdenum;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Mo].[Mo].[Bi+3].[Bi+3] DKUYEPUUXLQPPX-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 claims abstract description 51
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 33
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 33
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 26
- BYUANIDVEAKBHT-UHFFFAOYSA-N [Mo].[Bi] Chemical compound [Mo].[Bi] BYUANIDVEAKBHT-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000002245 particle Substances 0.000 claims abstract description 17
- 239000011247 coating layer Substances 0.000 claims abstract description 11
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 10
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 238000001354 calcination Methods 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 18
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 15
- 229910017604 nitric acid Inorganic materials 0.000 claims description 15
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 13
- 239000012065 filter cake Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000012153 distilled water Substances 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 239000002270 dispersing agent Substances 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- -1 aluminum alkoxide Chemical class 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 229910052750 molybdenum Inorganic materials 0.000 claims description 6
- 239000011733 molybdenum Substances 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 6
- 229910052720 vanadium Inorganic materials 0.000 claims description 6
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 6
- 239000011684 sodium molybdate Substances 0.000 claims description 5
- 235000015393 sodium molybdate Nutrition 0.000 claims description 5
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 5
- WOZZOSDBXABUFO-UHFFFAOYSA-N tri(butan-2-yloxy)alumane Chemical group [Al+3].CCC(C)[O-].CCC(C)[O-].CCC(C)[O-] WOZZOSDBXABUFO-UHFFFAOYSA-N 0.000 claims description 5
- 230000032683 aging Effects 0.000 claims description 4
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 4
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical group [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 claims description 4
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical group [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 3
- 239000011609 ammonium molybdate Substances 0.000 claims description 3
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 3
- 229940010552 ammonium molybdate Drugs 0.000 claims description 3
- 239000010410 layer Substances 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 229940068984 polyvinyl alcohol Drugs 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 3
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical group [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 claims description 3
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims description 2
- 229940113116 polyethylene glycol 1000 Drugs 0.000 claims description 2
- 229940085675 polyethylene glycol 800 Drugs 0.000 claims description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 2
- 230000004580 weight loss Effects 0.000 claims description 2
- 239000001054 red pigment Substances 0.000 claims 1
- 239000000049 pigment Substances 0.000 abstract description 33
- 239000002253 acid Substances 0.000 abstract description 11
- 239000007791 liquid phase Substances 0.000 abstract description 4
- 238000000576 coating method Methods 0.000 abstract description 3
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- 238000012360 testing method Methods 0.000 description 14
- 239000012071 phase Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 229910015667 MoO4 Inorganic materials 0.000 description 4
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- CJOBVZJTOIVNNF-UHFFFAOYSA-N cadmium sulfide Chemical compound [Cd]=S CJOBVZJTOIVNNF-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 239000001023 inorganic pigment Substances 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 238000001238 wet grinding Methods 0.000 description 2
- 229910002900 Bi2MoO6 Inorganic materials 0.000 description 1
- 229910002915 BiVO4 Inorganic materials 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 235000015895 biscuits Nutrition 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 230000002431 foraging effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- MOUPNEIJQCETIW-UHFFFAOYSA-N lead chromate Chemical compound [Pb+2].[O-][Cr]([O-])(=O)=O MOUPNEIJQCETIW-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
- 229910003158 γ-Al2O3 Inorganic materials 0.000 description 1
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/0006—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black containing bismuth and vanadium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
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- B82Y40/00—Manufacture or treatment of nanostructures
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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
本发明公开了一种超细氧化铝包裹型钼钒酸铋黄色颜料,由Al2O3透明壳体包裹层、以及包覆在其内的钼钒酸铋黄色颜料粉体颗粒构成。此外,还公开了上述超细氧化铝包裹型钼钒酸铋黄色颜料的制备方法。本发明超细氧化铝包裹型钼钒酸铋黄色颜料,通过三氧化二铝作为透明包裹壳体,包覆超细钼钒酸铋黄色颜料,显著提高了钼钒酸铋黄颜料的耐高温性和耐酸性,并能够满足更高的使用需求。本发明采用湿化学法在液相条件下制得的超细钼钒酸铋颗粒,在未经干燥、煅烧前即进行三氧化二铝包裹,避免了颜料粉体的团聚和结块,颜料颗粒粒径细且均匀、分散性好,并且无需昂贵的设备,工艺简单易操作、有助于推广和应用。
Description
技术领域
本发明涉及无机颜料技术领域,尤其涉及一种包裹型钼钒酸铋黄色颜料及其制备方法。
背景技术
镉黄(CdS)和铬黄(PbCrO4、BaCrO4),具有颜色鲜艳、遮盖力强、价格低廉等优点,是当下市面上普遍使用的无机黄色颜料,并且应用历史悠久、使用范围广。然而,由于所含的镉、铅和铬(VI)有毒金属元素会严重危害人类健康并污染环境,因此,开发新型的环保型黄色颜料以取而代之,不仅势在必行,更具有重要意义。
钼钒酸铋(通式为BiVO4·nBi2MoO6,0.2≤n≤2)是一种新型环保无毒的高级无机黄色颜料,其色调可通过n值的大小加以调控,当n值逐渐增大时,其色调由红相黄向绿相黄转变,当n=0.75时,即为已面市的BASF公司在颜料索引上注册的颜料黄PY184,它是由四方晶型的BiVO4和正交晶型的Bi2MoO6组成的亮绿色、遮盖力强的黄色无机颜料。
目前,钼钒酸铋黄色颜料的制造方法有直接煅烧法和沉淀-煅烧法。直接煅烧法是将相应氧化物或可经热分解而产生相应氧化物的盐按组成配料,经固相球磨混合后,在高温下煅烧。沉淀-煅烧法是先将相应可溶于水的各盐配料溶解,在相应的温度和pH等条件下使它们生成氧化物或氢氧化物凝胶沉淀,再将生成的沉淀进行洗涤、干燥后在约600℃温度下煅烧,最终形成相互毗邻的BiVO4和Bi2MoO6双相结晶。上述两种方法最后均须湿磨、抽滤以达到相应粒度,不仅工艺繁琐,而且所得颜料颗粒粒度仍然较大,难以满足更高的使用需求。
此外,现有技术上述颜料不耐强酸,并且煅烧到600℃以上时,颜料会因烧结而使颜色变深,失去亮黄色,因而不能在强酸环境下使用,亦不能应用于耐温性要求较高的领域,如工程塑料、高温涂料、玻璃油墨、陶瓷颜料等。因此,为提高颜料的使用性能,对钼钒酸铋黄色颜料进行表面改性处理已成为研究开发的热点,目前主要采用的方法均是在该颜料表面沉积无色无机物保护膜,如硅酸锆、磷酸盐及各种氧化物,但现有技术中色料颗粒与无机保护膜仅仅是互相混合吸附在一起,保护膜不够致密,因此效果并不理想。
发明内容
本发明的目的在于克服现有技术的不足,提供一种超细氧化铝包裹型钼钒酸铋黄色颜料,通过氧化铝作为透明包裹壳体,包覆超细钼钒酸铋黄色颜料,以显著提高钼钒酸铋黄色颜料的耐高温性和耐酸性,并满足更高的使用需求。本发明的另一目的在于提供上述超细氧化铝包裹型钼钒酸铋黄色颜料的制备方法,首先通过在液相条件下制得超细钼钒酸铋黄色颜料,然后不经干燥和煅烧,立即进行氧化铝包裹,从而获得超细、包裹致密的钼钒酸铋黄色颜料。
本发明的目的通过以下技术方案予以实现:
本发明提供的一种超细氧化铝包裹型钼钒酸铋黄色颜料,由Al2O3透明壳体包裹层、以及包覆在其内的钼钒酸铋黄色颜料粉体颗粒构成。所述超细氧化铝包裹型钼钒酸铋黄色颜料平均粒度为0.5~1.0μm,其中,所述Al2O3透明壳体包裹层的平均厚度为50~300nm。
上述方案中,本发明所述黄色颜料其红度值a*≤-3.0、黄度值b*≥70;在空气气氛下于1150℃煅烧后仍呈鲜艳明亮的黄色,其红度值a*≤-1.0、黄度值b*≥68;在釉料中氧化气氛下800℃煅烧后仍呈鲜艳明亮的黄色,其红度值a*≤0、黄度值b*≥60。所述黄色颜料经浓度为2mol/L的盐酸浸泡0.5h不变色,失重率<15wt%。
本发明的另一目的通过以下技术方案予以实现:
本发明提供的上述超细氧化铝包裹型钼钒酸铋黄色颜料的制备方法,包括以下步骤:
(1)超细钼钒酸铋黄色颜料滤饼的制备
(1-1)将硝酸铋(Bi(NO3)3·5H2O)溶解于硝酸溶液中,加入分散剂搅拌溶解后,得到A液;
(1-2)将钼源和钒源溶解于氢氧化钠溶液中,按照摩尔比Mo∶V∶Bi=2.50~2.80∶0.60~0.64∶1,得到B液;
(1-3)在室温下将所述A液和B液混合,调节溶液体系pH值为6.0~6.5,在搅拌和水浴条件下进行反应,然后经抽滤、洗涤,得到超细钼钒酸铋黄色颜料滤饼;
(2)Al2O3包裹钼钒酸铋黄色颜料的制备
(2-1)将所述超细钼钒酸铋黄色颜料滤饼分散到无水乙醇中,加入蒸馏水和浓硝酸搅拌后,按照摩尔比Al∶Bi=1~4∶1加入铝醇盐,在水浴条件下持续搅拌进行老化反应,反应后得到黄色溶胶;
(2-2)所述黄色溶胶经干燥、煅烧,冷却后即得到超细氧化铝包裹型钼钒酸铋黄色颜料。
本发明制备方法首先采用湿化学法在液相条件下制得亮黄色超细钼钒酸铋(Bi0.82V0.45Mo0.55O4),然后不经干燥和煅烧,利用铝醇盐的水解反应,在钼钒酸铋表面包裹致密的三氧化二铝,显著提高了颜料的耐高温性和耐酸性,从而获得超细的、耐高温耐酸钼钒酸铋黄色颜料。
进一步地,本发明制备方法所述分散剂为聚乙烯吡咯烷酮、十二烷基苯磺酸钠、十六烷基三甲基溴化铵、聚乙烯醇、聚乙二醇800、聚乙二醇1000,其用量为硝酸铋的5~8wt%。所述钼源为钼酸铵[(NH4)6Mo7O24·4H2O]、钼酸二钠(Na2MoO4·2H2O);所述钒源为偏钒酸钠(NaVO3)、偏钒酸铵(NH4VO3);所述铝醇盐为仲丁醇铝(3(C4H9O).Al)、异丙醇铝(C9H21AlO3)。
进一步地,本发明制备方法所述步骤(1-1)、(1-2)中硝酸和氢氧化钠溶液的浓度为1.5~2.5mol/L;所述步骤(1-3)水浴反应条件为:温度60~80℃、反应时间1.5~2.0h。所述步骤(2-1)中无水乙醇(C2H6O)的用量为按照摩尔比O∶Bi=100~150∶1;所述蒸馏水(H2O)的用量为按照摩尔比O∶Al=4~8∶1;所述浓硝酸(HNO3)的用量为按照摩尔比N∶Al=5~6∶1;所述老化反应的水浴温度为50~70℃,反应时间为1.0~6.0h。所述步骤(2-2)中干燥条件为:温度为室温~60℃,相对湿度25~35%;所述煅烧温度为800~900℃。
本发明具有以下有益效果:
(1)本发明超细氧化铝包裹型钼钒酸铋黄色颜料,其粒度小,平均粒度为0.5~1.0μm,能够满足更高的使用需求;其包裹体氧化铝,能够隔绝外界强酸腐蚀的同时,一方面极大地降低了颜料中Bi元素在高温下的挥发,确保了四方晶相钼钒酸铋(Bi0.82V0.45Mo0.55O4)的晶相稳定,从而大幅提升了颜料的高温稳定性;另一方面使颜料在高温下能够防止色料烧结变色。因此,本发明超细氧化铝包裹型钼钒酸铋黄色颜料耐强酸的同时,还可在1150℃高温煅烧和800℃熔块釉中煅烧后,依然保持颜色鲜艳,极大地拓展了其应用领域。
(2)本发明采用湿化学法在液相条件下制得的超细钼钒酸铋颗粒,在未经干燥、煅烧前即进行氧化铝包裹,避免了颜料粉体由于干燥、煅烧造成的团聚;同时,由于氧化铝的包裹,使颜料经800~900℃煅烧后不结块,因此,颜料颗粒很细,粒径均匀、分散性好,不需要经后续的湿磨、抽滤和烘干工艺,即可得到纳米级的黄色颜料粉体。
(3)本发明制备方法无需昂贵的设备,工艺简单易操作,影响因素易控制,有助于推广和应用。
附图说明
下面将结合实施例和附图对本发明作进一步的详细描述:
图1是本发明实施例一步骤(1-3)制得的超细钼钒酸铋黄色颜料滤饼经干燥后的透射电镜(TEM)照片;
图2是本发明实施例一制得的超细氧化铝包裹型钼钒酸铋黄色颜料的透射电镜(TEM)照片;
图3是本发明实施例一制得的超细氧化铝包裹型钼钒酸铋黄色颜料的XRD图谱。
具体实施方式
实施例一:
本实施例一种超细氧化铝包裹型钼钒酸铋黄色颜料的制备方法,其步骤如下:
(1)超细钼钒酸铋黄色颜料滤饼的制备
(1-1)将9.70g Bi(NO3)3·5H2O溶解于100mL浓度为2.0mol/L的硝酸溶液中,加入分散剂聚乙烯吡咯烷酮0.60g搅拌溶解后,得到A液;
(1-2)将9.76g钼酸铵[(NH4)6Mo7O24·4H2O]和1.48g偏钒酸钠(NaVO3)溶解于100mL浓度为2.0mol/L的氢氧化钠溶液中,得到B液;
(1-3)在室温下将上述A液和B液混合,用氢氧化钠溶液调节体系pH值为6.0,在搅拌和水浴温度为70℃条件下反应2.0h,经抽滤后,首先用大量蒸馏水洗涤一次,再用无水乙醇洗涤一次,得到超细钼钒酸铋黄色颜料滤饼(经干燥后的检测如图1所示,其分散性好,为不规则块状,粒径为100~200nm);
(2)Al2O3包裹钼钒酸铋黄色颜料的制备
(2-1)将上述超细钼钒酸铋黄色颜料滤饼分散到120mL无水乙醇中,加入4mL蒸馏水和12mL浓硝酸,搅拌0.5h后加入7.5mL仲丁醇铝,搅拌溶解后,水浴伴随持续搅拌升温至60±2℃进行老化反应2h,得到黄色溶胶;
(2-2)将上述黄色溶胶在60℃温度、30%相对湿度下干燥后,在800℃下煅烧,升温速度为5℃/min,保温时间为1h,冷却后即得到超细氧化铝包裹型钼钒酸铋(Bi0.82V0.45Mo0.55O4)黄色颜料。
如图2所示,本发明实施例一制得的超细氧化铝包裹型钼钒酸铋黄色颜料,由Al2O3透明壳体包裹层、以及包覆在其内的钼钒酸铋黄色颜料粉体颗粒构成,其分散性较好,形状不规则,粒径为0.5~1.0μm,其中,Al2O3透明壳体包裹层的平均厚度为50~300nm。
从图3可以看出,本发明实施例一制得的超细氧化铝包裹型钼钒酸铋黄色颜料为四方晶相Bi0.82V0.45Mo0.55O4(PDF 85-0631),颜料的包裹层为γ-Al2O3(PDF10-0425)。
实施例二:
本实施例一种超细氧化铝包裹型钼钒酸铋黄色颜料的制备方法,其步骤如下:
(1)超细钼钒酸铋黄色颜料滤饼的制备
(1-1)将7.30g Bi(NO3)3·5H2O溶解于100mL浓度为1.5mol/L的硝酸溶液中,加入分散剂聚乙烯醇0.45g搅拌溶解后,得到A液;
(1-2)将10.0g钼酸二钠(Na2MoO4·2H2O)和1.06g偏钒酸铵(NH4VO3)溶解于100mL浓度为1.5mol/L的氢氧化钠溶液中,得到B液;
(1-3)在室温下将上述A液和B液混合,用氢氧化钠溶液调节体系pH值为6.5,在搅拌和水浴温度为70℃条件下反应2.0h,经抽滤后,首先用大量蒸馏水洗涤一次,再用无水乙醇洗涤一次,得到超细钼钒酸铋黄色颜料滤饼;
(2)Al2O3包裹钼钒酸铋黄色颜料的制备
(2-1)将上述超细钼钒酸铋黄色颜料滤饼分散到120mL无水乙醇中,加入3mL蒸馏水和10mL浓硝酸,搅拌0.5h后加入5.5g异丙醇铝,搅拌溶解后,水浴伴随持续搅拌升温至60±2℃进行老化反应3h,得到黄色溶胶;
(2-2)将上述黄色溶胶在50℃温度、25%相对湿度下干燥后,在900℃下煅烧,升温速度为5℃/min,保温时间为1h,冷却后即得到超细氧化铝包裹型钼钒酸铋(Bi0.82V0.45Mo0.55O4)黄色颜料。
实施例三:
本实施例一种超细氧化铝包裹型钼钒酸铋黄色颜料的制备方法,与实施例一不同之处在于:
步骤(1-2)中钒源为偏钒酸铵(NH4VO3),用量为1.42g;
步骤(1-3)中水浴温度为65℃;
步骤(2-1)中浓硝酸的用量为14mL,仲丁醇铝的用量为9.5mL。
实施例四:
本实施例一种超细氧化铝包裹型钼钒酸铋黄色颜料的制备方法,与实施例一不同之处在于:
步骤(1-2)中钼源为钼酸二钠(Na2MoO4·2H2O),用量为13.38g;钒源为偏钒酸铵(NH4VO3),用量为1.42g;
步骤(2-1)中无水乙醇用量为80mL,浓硝酸的用量为9mL,蒸馏水的用量为3mL,仲丁醇铝的用量为6.0mL,煅烧温度为900℃。
实施例五:
本实施例一种超细氧化铝包裹型钼钒酸铋黄色颜料的制备方法,与实施例二不同之处在于:
步骤(1-1)中Bi(NO3)3·5H2O的用量为9.70g;
步骤(1-2)中钼酸二钠(Na2MoO4·2H2O)的用量为12.9g;偏钒酸铵(NH4VO3)的用量为1.45g;
步骤(2-1)中浓硝酸的用量为12mL,异丙醇铝的用量为7.0g。
性能测试:
1、色度参数测试:采用杭州研特科技有限公司生产的YT-ACM402全自动色度仪进行测试:模拟D65照明体照明,采用d/0照明观测几何条件,漫射球直径为150mm,测试孔直径为30mm,测试波长范围为可见光(400~700nm),测其颜料的色度参数CIE-L*a*b*,其中L*代表由黑(0)到白(100),a*表示由绿色(-)到红色(+),b*表示由蓝色(-)到黄色(+)。
2、耐酸性测试:精确称取0.1000g色料置于干燥的离心试管中,加入10mL浓度为2mol/L的盐酸浸泡半小时,离心,小心将清液倾倒丢弃,用酒精离心洗涤两次,烘干称重,计算酸蚀失量(wt%)=(G0-G1)/G0×100%,其中G0、G1分别为盐酸浸泡前、后色料重量。
3、耐温性测试:
(1)裸烧耐温性测试:将色料置于氧化铝坩埚中,在空气气氛中于某一温度点保温煅烧1h,冷却后测其色度参数。
(2)低温熔块釉中耐温性测试:
取色料粉体0.5g,与1.5g低温熔块(Al2O3-B2O3-SiO2-ZnO体系)粉体和4mL去离子水研磨混合均匀形成釉浆,将之均匀涂覆于已经烧成的陶瓷素坯上,干燥后以10℃/min升温至800℃,保温10min,随炉冷却后测其色度参数。
本发明各实施例制得的超细氧化铝包裹型钼钒酸铋黄色颜料的色度参数如表1所示。
以实施例一步骤(1-3)制得的超细钼钒酸铋黄色颜料滤饼经干燥后的黄色颜料(即未包裹的超细钼钒酸铋黄色颜料)作为对比例。该对比例、以及本发明各实施例所制得的黄色颜料的耐酸性测试值如表2所示,裸烧耐温性测试结果如表3所示,在低温熔块釉中的耐温性测试结果如表4所示。
表1本发明各实施例制得的超细氧化铝包裹型钼钒酸铋黄色颜料的色度参数
表2本发明各实施例和对比例的耐酸性测试值
表3本发明各实施例和对比例在空气气氛中煅烧后的色度参数
表4本发明各实施例和对比例在低温熔块中煅烧后的色度参数
Claims (7)
1.一种超细氧化铝包裹型钼钒酸铋黄色颜料的制备方法,其特征在于包括以下步骤:
(1) 超细钼钒酸铋黄色颜料滤饼的制备
(1-1) 将硝酸铋溶解于硝酸溶液中,加入分散剂搅拌溶解后,得到A液;其中,所述分散剂为聚乙烯吡咯烷酮、十二烷基苯磺酸钠、十六烷基三甲基溴化铵、聚乙烯醇、聚乙二醇800、聚乙二醇1000,其用量为硝酸铋的5~8 wt%;
(1-2) 将钼源和钒源溶解于氢氧化钠溶液中,按照摩尔比Mo∶V∶Bi=2.50~2.80∶0.60~0.64∶1,得到B液;
(1-3) 在室温下将所述A液和B液混合,调节溶液体系pH值为6.0~6.5,在搅拌、60~80℃温度下水浴反应1.5~2.0 h,然后经抽滤、洗涤,得到超细钼钒酸铋黄色颜料滤饼;
(2) Al2O3包裹钼钒酸铋黄色颜料的制备
(2-1) 将所述超细钼钒酸铋黄色颜料滤饼分散到无水乙醇中,加入蒸馏水和浓硝酸搅拌后,按照摩尔比Al∶Bi=1~4∶1加入铝醇盐,在水浴温度为50~70 ℃条件下持续搅拌进行老化反应1.0~6.0 h,反应后得到黄色溶胶;其中,所述无水乙醇的用量为按照摩尔比O∶Bi=100~150∶1,所述蒸馏水的用量为按照摩尔比O∶Al=4~8∶1,所述浓硝酸的用量为按照摩尔比N∶Al=5~6∶1;
(2-2) 所述黄色溶胶经干燥后,在800~900℃温度下煅烧,冷却后即得到超细氧化铝包裹型钼钒酸铋黄色颜料,所述钼钒酸铋为四方晶相钼钒酸铋Bi0.82V0.45Mo0.55O4。
2.根据权利要求1所述的超细氧化铝包裹型钼钒酸铋黄色颜料的制备方法,其特征在于:所述钼源为钼酸铵、钼酸二钠;所述钒源为偏钒酸钠、偏钒酸铵;所述铝醇盐为仲丁醇铝、异丙醇铝。
3.根据权利要求1所述的超细氧化铝包裹型钼钒酸铋黄色颜料的制备方法,其特征在于:所述步骤(1-1)、(1-2)中硝酸和氢氧化钠溶液的浓度为1.5~2.5 mol/L。
4.根据权利要求1所述的超细氧化铝包裹型钼钒酸铋黄色颜料的制备方法,其特征在于:所述步骤(2-2)中干燥条件为:温度为室温~60℃,相对湿度25~35%。
5.根据权利要求1所述的超细氧化铝包裹型钼钒酸铋黄色颜料的制备方法,其特征在于:所述超细氧化铝包裹型钼钒酸铋黄色颜料由Al2O3透明壳体包裹层、以及包覆在其内的钼钒酸铋黄色颜料粉体颗粒构成;所述超细氧化铝包裹型钼钒酸铋黄色颜料平均粒度为0.5~1.0 mm,其中,所述Al2O3透明壳体包裹层的平均厚度为50~300 nm。
6.根据权利要求1或5所述的超细氧化铝包裹型钼钒酸铋黄色颜料的制备方法,其特征在于:所述超细氧化铝包裹型钼钒酸铋黄色颜料其红度值a*≤-3.0、黄度值b*≥70;在空气气氛下于1150℃煅烧后仍呈鲜艳明亮的黄色,其红度值a*≤-1.0、黄度值b*≥68;在釉料中氧化气氛下800℃煅烧后仍呈鲜艳明亮的黄色,其红度值a*≤0、黄度值b*≥60。
7.根据权利要求1或5所述的超细氧化铝包裹型钼钒酸铋黄色颜料的制备方法,其特征在于:所述超细氧化铝包裹型钼钒酸铋黄色颜料经浓度为2 mol/L的盐酸浸泡0.5 h不变色,失重率<15 wt%。
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