CN106752112B - 一种高近红外反射比钛黄的生产方法 - Google Patents

一种高近红外反射比钛黄的生产方法 Download PDF

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CN106752112B
CN106752112B CN201611150510.2A CN201611150510A CN106752112B CN 106752112 B CN106752112 B CN 106752112B CN 201611150510 A CN201611150510 A CN 201611150510A CN 106752112 B CN106752112 B CN 106752112B
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谢宏伟
廖向阳
王玲
杨伟伟
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Jiangsu New Mstar Technology Ltd
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Abstract

本发明公开了一种高近红外反射比钛黄的生产方法。本发明利用纳米级水合二氧化钛的高反应活性,选用合适的纳米级水合二氧化钛,添加正钛酸溶胶、锌元素、氧化锑、磷酸、氧化镍等添加剂,经过高温煅烧,粉碎,除盐制得高近红外反射比钛黄产品。该产品具有合理的粒径分布、颜色适中、易分散、近红外反射比高的显著特征,是黄色近红外反射功能材料的理想产品。

Description

一种高近红外反射比钛黄的生产方法
技术领域
本发明涉及钛黄的制法,尤其是涉及利用合适的纳米级水合二氧化钛制备高近红外反射比钛黄的生产方法。
背景技术
目前国内外对节能技术日趋重视,提高对太阳辐射的直接反射能力是一种简便易行的技术路线。从太阳的能量分布来看,地球上所能接收到的太阳辐射能的波长主要分布在250~2500nm范围内,可将其分成三个部分,每个部分的波长范围和所占能量分别为:小于380nm的紫外光区约占总能量的3%;380~780nm的可见光区约占总能量的45%;大于780nm的近红外区约占总能量的52%。产生热效应的主要太阳辐射能的波长为大于780nm的近红外区,提高对近红外区太阳辐射能的直接反射,能起到降温降耗的效果。
传统的彩色颜料,不能适应节能要求的高近红外反射能力,不能满足节能型功能产品应用要求。具有金红石型晶型结构的钛黄当控制到合理的粒径分布时,则能有高的近红外反射比,是较理想的彩色近红外反射功能材料之一。
钛黄具有的优异性能:1.由于通过高温反应和煅烧得来,具有金红石型晶型,晶格结构稳定,耐热、耐光、耐候和耐各种化学介质性能非常优良,抗粉化性能良好。2.钛黄具有中性的PH值,适用于各种介质体系,不会与介质体系起反应。3.钛黄含有的发色元素进入TiO2晶格,一般条件下不被任何介质浸蚀,完全适用于无毒无害化要求的安全体系。
市场上较成熟的钛黄产品多采用固相法工艺,以钛白粉为主要原料,虽然工艺较为简单,成本较低,但由于钛白粉已经是稳定的晶体结构,需要较高的温度进行固体氧化物混合煅烧,导致产品质量不稳定。利用纳米级高活性水合二氧化钛为主要原料进行钛黄的生产,物料之间实现分子级别的混合,是一种简便易行且产品质量稳定可控的生产方法。
发明内容
本发明的目的,是为了提供一种高近红外反射比钛黄的生产方法,该方法解决的技术问题是利用纳米级水合二氧化钛的高反应活性的特点,实现物料之间是分子级别的混合。通过优选纳米级高活性水合二氧化钛、对水合二氧化钛进行一次水洗、酸处理、二次水洗、加处理剂混合、煅烧、一次粉碎、研磨除盐、干燥、汽流粉碎等主要步骤,以达到产出高近红外反射比钛黄的目的。
本发明提供的生产方法包括下述步骤:
a、水合二氧化钛一次水洗:选取硫酸法钛白生产工艺制备的水解产物水合二氧化钛,沉降率指标符合150~200mm/20min,以55~70℃自来水对水合二氧化钛进行水洗,水洗合格的判定指标为一次水洗废水中的铁含量(以Fe计)小于100mg/L;
b、酸处理:将一次水洗所得水合二氧化钛加自来水制成浆料,浓度控制为320~380g/L,温度在55~70℃,加入硫酸(以H2SO4计)为30~50g/L,三价钛(以Ti2O3计)为0.5~1.5g/L,在此条件下处理浆料1~2小时;处理结束后,加入煅烧晶种,煅烧晶种中TiO2的质量以占待处理浆料中所含TiO2质量2~7%,搅拌30分钟;
所述煅烧晶种为正钛酸溶胶煅烧晶种,所述正钛酸溶胶煅烧晶种为硫酸法钛白生产工艺制备的金红石型煅烧晶种。
c、水合二氧化钛二次水洗:以55~70℃脱盐水对步骤b酸处理好的水合二氧化钛浆料进行水洗,水洗合格的判定指标为二次水洗废水中的铁含量(以Fe2O3计)控制在小于10mg/L。
d、加处理剂:将二次水洗所得水合二氧化钛浆料加脱盐水调节二氧化钛浓度控制为320~380g/L;用碱调整浆料PH值到2.5~4.0;以占待处理浆料中所含TiO2量的质量分数计,以Sb2O3计,加入的氧化锑添加比例为10~15%;以NiO计,氧化镍添加比例为5~10%;以H3PO4计,磷酸添加比例为0.00~0.25%;以ZnO计,氧化锌或硫酸锌或氯化锌添加比例为0.0~0.5%;以MgO计,氧化镁或硫酸镁或氯化镁添加比例为0.0~0.5%;加完上述试剂后搅拌浆料0.5~1小时,将浆料压干水份备用。
e、煅烧:将压干水份的物料进行煅烧,最高煅烧温度控制在900~1200℃之间,煅烧品中金红石型晶型含量≥98.5%;
f、粉碎:将煅烧品用粉碎机进行粉碎,控制粉碎细度45μm筛余物小于0.05%,即得高近红外反射比钛黄初级产品;
g、除盐、砂磨:将钛黄初级产品用脱盐水制成浆料,用砂磨机对浆料进行研磨,选用1.2~1.4μm的硅酸锆珠或钇稳定锆珠,用脱盐水对研磨后的浆料进行水洗,控制水洗废水电导率小于80μm/cm,将浆料压干水分备用;
h、干燥、汽流粉碎:将压干水分的物料烘干去除水分,加入三羟甲基乙烷、三羟甲基丙烷、聚二甲基硅氧烷聚合物其中的一种,添加量为占粉碎物料质量的0.1~0.8%,经汽流粉碎得钛黄产品。
本发明的有益效果为:
(1)本发明所得产品为金红石型晶体结构,具有理想的粒径分布,粒径D50介于500~1500nm之间,产品具有优异近红外线反射能力。该方法通过优选纳米级高活性水合二氧化钛并经过对其进行除杂后再加入发色元素、助剂,实现物料之间是分子级别的混合,使得钛黄产品的粒径可控成长;通过对初级产品进行除盐、研磨、并加入不同的表面活性剂,可使得产品具有更广泛的适用性。
(2)本发明工艺简单,操作方便,成本低廉。
附图说明
附图1是实施例1和市售产品的光反射曲线图。
具体实施方式
下面结合附图以及具体实施例对本发明作进一步的说明,但本发明的保护范围并不限于此。
实施例1
取硫酸法钛白生产工艺制备的水解产物水合二氧化钛,沉降率为150mm/20min,以60~65℃自来水对水合二氧化钛进行水洗,一次水洗废水中的铁含量(以Fe计)95mg/L;将一次水洗所得水合二氧化钛加自来水制成浆料,浓度为325g/L,温度在60~65℃,加入硫酸(以H2SO4计)为49g/L,三价钛(以Ti2O3计)为0.5g/L,处理2小时后以占待处理浆料中所含TiO2量的质量分数计,加入正钛酸溶胶煅烧晶种(以TiO2计),添加比例为5%;以55~60℃脱盐水对酸处理好的水合二氧化钛进行水洗,二次水洗废水中的铁含量(以Fe2O3计)为8mg/L;将二次水洗所得水合二氧化钛加脱盐水制成浆料,浓度为330g/L;用氢氧化钾调整浆料PH值到2.5~4.0;以占待处理浆料中所含TiO2量的质量分数计,加入的氧化锑(以Sb2O3计)添加比例为11%;氧化镍(以NiO计)添加比例为6%;氧化锌或硫酸锌或氯化锌(以ZnO计)添加比例为0.5%;加完上述试剂后搅拌0.5~1小时,将浆料压干水分进行煅烧,最高煅烧温度控制在1000℃,煅烧品中金红石型晶型含量为99.5%;将煅烧品用机械粉碎机进行粉碎,粉碎细度0.05%,即得高近红外反射比钛黄初级产品;将钛黄初级产品用脱盐水制成浆料,用砂磨机对浆料进行研磨,选用1.2~1.4μm的硅酸锆珠,用脱盐水对研磨后的浆料进行水洗,水洗废水电导率75μm/cm,将浆料压干水分;将压干水分的物料烘干去除水分,加入三羟甲基乙烷,添加量为占粉碎物料质量的0.2%,经汽流粉碎得高近红外反射比钛黄产品。
实施例2
取硫酸法钛白生产工艺制备的水解产物水合二氧化钛,沉降率为197mm/20min,以55~60℃自来水对水合二氧化钛进行水洗,一次水洗废水中的铁含量(以Fe计)85mg/L;将一次水洗所得水合二氧化钛加自来水制成浆料,浓度为372g/L,温度在55~60℃,加入硫酸(以H2SO4计)为32g/L,三价钛(以Ti2O3计)为1.5g/L,处理1.5小时后以占待处理浆料中所含TiO2量的质量分数计,加入正钛酸溶胶煅烧晶种(以TiO2计),添加比例为7%;以60~65℃脱盐水对酸处理好的水合二氧化钛进行水洗,二次水洗废水中的铁含量(以Fe2O3计)为10mg/L;将二次水洗所得水合二氧化钛加脱盐水制成浆料,浓度为378g/L;用碳酸钾调整浆料PH值到2.5~4.0;以占待处理浆料中所含TiO2量的质量分数计,加入的氧化锑(以Sb2O3计)添加比例为15%;氧化镍(以NiO计)添加比例为10%;磷酸(以H3PO4计)添加比例为0.00%;氧化锌或硫酸锌或氯化锌(以ZnO计)添加比例为0.0%;氧化镁或硫酸镁或氯化镁添加比例为0.5%;加完上述试剂后搅拌0.5~1小时,将浆料压干水分进行煅烧,最高煅烧温度控制在980℃,煅烧品中金红石型晶型含量为98.5%;将煅烧品用机械粉碎机进行粉碎,粉碎细度0.04%,即得高近红外反射比钛黄初级产品;将钛黄初级产品用脱盐水制成浆料,用砂磨机对浆料进行研磨,选用1.2~1.4μm的钇稳定锆珠,用脱盐水对研磨后的浆料进行水洗,水洗废水电导率75μm/cm,将浆料压干水分;将压干水分的物料烘干去除水分,加入三羟甲基丙烷,添加量为占粉碎物料质量的0.4%,经汽流粉碎得高近红外反射比钛黄产品。
实施例3
取硫酸法钛白生产工艺制备的水解产物水合二氧化钛,沉降率为175mm/20min,以55~60℃自来水对水合二氧化钛进行水洗,一次水洗废水中的铁含量(以Fe计)85mg/L;将一次水洗所得水合二氧化钛加自来水制成浆料,浓度为365g/L,温度在65~70℃,加入硫酸(以H2SO4计)为38g/L,三价钛(以Ti2O3计)为1.1g/L,处理1小时后以占待处理浆料中所含TiO2量的质量分数计,加入正钛酸溶胶煅烧晶种(以TiO2计),添加比例为2%;以55~60℃脱盐水对酸处理好的水合二氧化钛进行水洗,二次水洗废水中的铁含量(以Fe2O3计)为9mg/L;将二次水洗所得水合二氧化钛加脱盐水制成浆料,浓度控制为370g/L;用氢氧化钠调整浆料PH值到2.5~4.0;以占待处理浆料中所含TiO2量的质量分数计,加入的氧化锑(以Sb2O3计)添加比例为12%;氧化镍(以NiO计)添加比例为8%;磷酸(以H3PO4计)添加比例为0.20%;氧化锌或硫酸锌或氯化锌(以ZnO计)添加比例为0.4%;氧化镁或硫酸镁或氯化镁添加比例为0.2%;加完上述试剂后搅拌0.5~1小时,将浆料压干水分进行煅烧,最高煅烧温度控制在1100℃,煅烧品中金红石型晶型含量≥99.0%;将煅烧品用机械粉碎机进行粉碎,粉碎细度0.04%,即得高近红外反射比钛黄初级产品;将钛黄初级产品用脱盐水制成浆料,用砂磨机对浆料进行研磨,选用1.2~1.4μm的硅酸锆珠,用脱盐水对研磨后的浆料进行水洗,水洗废水电导率80μm/cm,将浆料压干水分;将压干水分的物料烘干去除水分,加入聚二甲基硅氧烷聚合物,添加量为占粉碎物料质量的0.8%,经汽流粉碎得高近红外反射比钛黄产品。
对实施例的钛黄产品进行检测,其中的R%为XRD检测结果,粒径为激光粒度仪检测结果,近红外反射比(NIR)为安捷伦cary 5000检测结果,所得检测数据在后文表1中列示:
表1:实施例产品检测数据

Claims (4)

1.一种高近红外反射比钛黄的生产方法,其特征在于,包括以下步骤:取硫酸法钛白生产工艺制备的水解产物水合二氧化钛,沉降率为150mm/20min,以60~65℃自来水对水合二氧化钛进行水洗,一次水洗废水中的铁含量以Fe计95mg/L;将一次水洗所得水合二氧化钛加自来水制成浆料,浓度为325g/L,温度在60~65℃,加入硫酸以H2SO4计为49g/L,三价钛以Ti2O3计为0.5g/L,处理2小时后以占待处理浆料中所含TiO2量的质量分数计,加入正钛酸溶胶煅烧晶种以TiO2计,添加比例为5%;以55~60℃脱盐水对酸处理好的水合二氧化钛进行水洗,二次水洗废水中的铁含量以Fe2O3计为8mg/L;将二次水洗所得水合二氧化钛加脱盐水制成浆料,浓度为330g/L;用氢氧化钾调整浆料PH值到2.5~4.0;以占待处理浆料中所含TiO2量的质量分数计,加入的氧化锑以Sb2O3计添加比例为11%;氧化镍以NiO计添加比例为6%;氧化锌或硫酸锌或氯化锌以ZnO计添加比例为0.5%;加完上述试剂后搅拌0.5~1小时,将浆料压干水分进行煅烧,最高煅烧温度控制在1000℃,煅烧品中金红石型晶型含量为99.5%;将煅烧品用机械粉碎机进行粉碎,粉碎细度0.05%,即得高近红外反射比钛黄初级产品;将钛黄初级产品用脱盐水制成浆料,用砂磨机对浆料进行研磨,选用1.2~1.4μm的硅酸锆珠,用脱盐水对研磨后的浆料进行水洗,水洗废水电导率75μm/cm,将浆料压干水分;将压干水分的物料烘干去除水分,加入三羟甲基乙烷,添加量为占粉碎物料质量的0.2%,经汽流粉碎得高近红外反射比钛黄产品。
2.一种高近红外反射比钛黄的生产方法,其特征在于,包括以下步骤:取硫酸法钛白生产工艺制备的水解产物水合二氧化钛,沉降率为197mm/20min,以55~60℃自来水对水合二氧化钛进行水洗,一次水洗废水中的铁含量以Fe计85mg/L;将一次水洗所得水合二氧化钛加自来水制成浆料,浓度为372g/L,温度在55~60℃,加入硫酸以H2SO4计为32g/L,三价钛以Ti2O3计为1.5g/L,处理1.5小时后以占待处理浆料中所含TiO2量的质量分数计,加入正钛酸溶胶煅烧晶种以TiO2计,添加比例为7%;以60~65℃脱盐水对酸处理好的水合二氧化钛进行水洗,二次水洗废水中的铁含量以Fe2O3计为10mg/L;将二次水洗所得水合二氧化钛加脱盐水制成浆料,浓度为378g/L;用碳酸钾调整浆料PH值到2.5~4.0;以占待处理浆料中所含TiO2量的质量分数计,加入的氧化锑以Sb2O3计添加比例为15%;氧化镍以NiO计添加比例为10%;磷酸以H3PO4计添加比例为0.00%;氧化镁或硫酸镁或氯化镁添加比例为0.5%;加完上述试剂后搅拌0.5~1小时,将浆料压干水分进行煅烧,最高煅烧温度控制在980℃,煅烧品中金红石型晶型含量为98.5%;将煅烧品用机械粉碎机进行粉碎,粉碎细度0.04%,即得高近红外反射比钛黄初级产品;将钛黄初级产品用脱盐水制成浆料,用砂磨机对浆料进行研磨,选用1.2~1.4μm的钇稳定锆珠,用脱盐水对研磨后的浆料进行水洗,水洗废水电导率75μm/cm,将浆料压干水分;将压干水分的物料烘干去除水分,加入三羟甲基丙烷,添加量为占粉碎物料质量的0.4%,经汽流粉碎得高近红外反射比钛黄产品。
3.一种高近红外反射比钛黄的生产方法,其特征在于,包括以下步骤:取硫酸法钛白生产工艺制备的水解产物水合二氧化钛,沉降率为175mm/20min,以55~60℃自来水对水合二氧化钛进行水洗,一次水洗废水中的铁含量以Fe计85mg/L;将一次水洗所得水合二氧化钛加自来水制成浆料,浓度为365g/L,温度在65~70℃,加入硫酸以H2SO4计为38g/L,三价钛以Ti2O3计为1.1g/L,处理1小时后以占待处理浆料中所含TiO2量的质量分数计,加入正钛酸溶胶煅烧晶种以TiO2计,添加比例为2%;以55~60℃脱盐水对酸处理好的水合二氧化钛进行水洗,二次水洗废水中的铁含量以Fe2O3计为9mg/L;将二次水洗所得水合二氧化钛加脱盐水制成浆料,浓度控制为370g/L;用氢氧化钠调整浆料PH值到2.5~4.0;以占待处理浆料中所含TiO2量的质量分数计,加入的氧化锑以Sb2O3计添加比例为12%;氧化镍以NiO计添加比例为8%;磷酸以H3PO4计添加比例为0.20%;氧化锌或硫酸锌或氯化锌以ZnO计添加比例为0.4%;氧化镁或硫酸镁或氯化镁添加比例为0.2%;加完上述试剂后搅拌0.5~1小时,将浆料压干水分进行煅烧,最高煅烧温度控制在1100℃,煅烧品中金红石型晶型含量≥99.0%;将煅烧品用机械粉碎机进行粉碎,粉碎细度0.04%,即得高近红外反射比钛黄初级产品;将钛黄初级产品用脱盐水制成浆料,用砂磨机对浆料进行研磨,选用1.2~1.4μm的硅酸锆珠,用脱盐水对研磨后的浆料进行水洗,水洗废水电导率80μm/cm,将浆料压干水分;将压干水分的物料烘干去除水分,加入聚二甲基硅氧烷聚合物,添加量为占粉碎物料质量的0.8%,经汽流粉碎得高近红外反射比钛黄产品。
4.根据权利要求1-3中任一项所述的制备方法制得的高近红外反射比钛黄的用途,其特征在于,将所述高近红外反射比钛黄产品用于需要反射近红外线的黄色体系。
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