WO2013020427A1 - 低浓度钛液制备高亮度金红石钛白粉的水解方法 - Google Patents

低浓度钛液制备高亮度金红石钛白粉的水解方法 Download PDF

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WO2013020427A1
WO2013020427A1 PCT/CN2012/078161 CN2012078161W WO2013020427A1 WO 2013020427 A1 WO2013020427 A1 WO 2013020427A1 CN 2012078161 W CN2012078161 W CN 2012078161W WO 2013020427 A1 WO2013020427 A1 WO 2013020427A1
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titanium
concentration
hydrolysis
boiling
heating
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PCT/CN2012/078161
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French (fr)
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林发蓉
陈刚
蔡平雄
邓伯松
朱全芳
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四川龙蟒钛业股份有限公司
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Publication of WO2013020427A1 publication Critical patent/WO2013020427A1/zh

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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00Compounds of titanium
    • C01G23/04Oxides; Hydroxides
    • C01G23/047Titanium dioxide
    • C01G23/053Producing by wet processes, e.g. hydrolysing titanium salts

Definitions

  • the invention relates to a hydrolysis method for preparing high-brightness rutile titanium dioxide by hydrolysis of a low concentration titanium liquid by spontaneous seeding in a production process of titanium dioxide produced by a sulfuric acid process.
  • titanium dioxide produced by sulfuric acid method the main factor determining the quality of titanium white product is the choice of hydrolysis process.
  • the quality of hydrolysis not only affects the economics of industrial production, but also has a great relationship to the quality of the final product.
  • sulfuric acid rutile titanium dioxide has soil properties such as whiteness and brightness. Because it has more colored impurities in sulfuric acid titanium dioxide, it also exists in particle size, distribution and morphology. A big gap.
  • the seed crystal is diluted and hydrolyzed. Because the amount of bottom water is large, it is generally 1: (3.5-4), which requires a very high concentration of titanium liquid. Many patents require 220g/L or more (or even 250-260 g L). Thus, in the whole titanium white production process, the concentration position becomes one of the production bottlenecks, especially in the winter with low temperature, the concentration rate is slow, the steam consumption is high, the production of titanium liquid is limited, and finally the whole production capacity is affected.
  • the present invention optimizes the hydrolysis scheme, does not increase the process, does not add equipment, appropriately reduces the amount of bottom water, reduces the concentration of titanium liquid, improves the washing property of the hydrolyzate, improves the impurity content in the metatitanic acid, and improves the particle morphology of the product. It can improve the performance of pigments such as whiteness and brightness, and at the same time achieve the purpose of reducing production costs.
  • the object of the present invention is to overcome the above drawbacks, and provide a hydrolysis method for preparing high-intensity rutile titanium dioxide by low-concentration titanium liquid, and reducing the concentration of titanium liquid and reducing the amount of bottom water on the basis of the existing autogenous seed hydrolysis technology.
  • the new hydrolysis method saves concentrated steam, reduces production costs, and improves product quality.
  • a method for preparing high-brightness rutile titanium dioxide by low-concentration titanium liquid comprises the following steps: a. adding preheated bottom water to the hydrolysis pot; b, taking preheated titanium liquid and slowly adding to the bottom water , c, heating the material obtained in step b to boiling, and maintaining the micro-boiling state until the material becomes steel gray, then stop heating and reduce the stirring speed; d, heat the material again to a slight boiling, and maintain the micro-boiling state for 20 to 35 min ; e.
  • step b Concentration is 190 ⁇ 215g / L; volume ratio of bottom water to titanium liquid 1: (4.5 ⁇ 6).
  • the bottom water and the titanium liquid are each preheated to 90 to 98 ° C, and the titanium liquid in step b may be a titanium liquid which is acid-decomposed or precipitated by titanium concentrate, or may be acid solution by using high-titanium slag.
  • the sedimentation filtered titanium liquid, the mass ratio of Fe/Ti0 2 in the titanium liquid is controlled at 0.25 ⁇ 0.35, and the preheating is generally carried out by steam heating; the preheated titanium liquid is added to the bottom water in 15 ⁇ 25min, step c
  • the material is heated to boiling in 20 ⁇ 25 min; and the dilution concentration of the titanium liquid in step e can refer to the parameters of the existing titanium liquid hydrolysis process.
  • the concentration of titanium solution is not a major factor in the quality of the product when it is hydrolyzed, it is determined by the initial concentration of titanium but by the concentration of titanium and the amount of bottom water.
  • the same titanium concentration decreases with the increase of the bottom water amount; the same bottom water amount increases with the increase of the titanium liquid concentration.
  • the amount of bottom water determines the quantity and quality of the hydrolyzed seed crystals, determines the quality of the metatitanic acid, and ultimately determines the quality of the product.
  • the primary particles of hydrated titanium dioxide are finer.
  • the surface free energy of the fine particles is large, it is easy to flocculate into large particles and settle down. The speed is fast and the time is short, but the washing time is too short to form a washing short circuit, which is not conducive to the washing of impurities such as iron, affecting whiteness, brightness and achromatic power.
  • concentration of titanium solution is too low, and the initial concentration of hydrolysis is ensured, the amount of bottom water added is too small, then the number of crystallization centers is small, the hydrolysis rate is slow, and the primary primary particles of hydrated titanium dioxide are coarse, which is not conducive to flocculation of the hydrolyzed material and affects washing; The hydrolysis rate is low and the yield is low; and the final product has poor performance such as whiteness and brightness. Therefore, selecting the appropriate concentration and amount of bottom water, controlling the appropriate amount of seed crystals, the appropriate hydrolysis rate, and the suitable primary particles of hydrated titanium dioxide can help improve the washing effect and improve product quality.
  • the process controls the concentration of the titanium liquid, the amount of the titanium liquid, and the ratio of the amount of the bottom water, thereby optimizing the hydrolysis process, improving the washing effect, and improving the product quality.
  • concentration is one of the bottlenecks, because the higher the concentration of titanium solution, the greater the concentration pressure, the titanium solution concentration is generally above 220g / L, the average evaporation It water consumes It steam. If the concentration of titanium liquid is reduced to 205g/L, the production of It (folded Ti0 2 ) titanium liquid can save 0.38 tons of steam, plus the heating steam consumed by the bottom water can achieve 50 yuan / Tons of cost savings.
  • the process reduces the concentration of the titanium liquid, reduces the amount of the bottom water, ensures the hydrolysis effect, and eliminates the need for steam concentration and other process steps in the process, thereby saving costs.
  • the volume ratio of the bottom water to the titanium liquid is 1: (5 ⁇ 5.5).
  • the amount of bottom water is affecting the washing effect of the hydrolyzed material. The most important factor, the amount of bottom water mainly affects the number of seed crystals, the number of crystal seeds is large, the number of crystal centers is large, and the primary primary particles of hydrated titanium dioxide are fine. Because the surface free energy of fine particles is large, it is easy to flocculate into large particles and settle down. The washing speed is fast and the time is short, but the washing time is too short to form a washing short circuit and is not conducive to iron washing. In the process, the optimal bottom water amount is 1: (5 5.5).
  • the method of the invention is an improvement on the existing titanium liquid hydrolysis process, and can reduce the concentration of the concentrated titanium liquid and reduce the amount of the bottom water without increasing any process, without adding any equipment investment, but can improve the washing of the hydrolysis material.
  • Improves the content of impurities in metatitanic acid improves the particle morphology of the product, improves the performance of pigments such as whiteness and brightness, improves product quality and productivity, greatly reduces production costs, and is practical in industrial applications.
  • 1500ml concentrated titanium liquid with a concentration of 190g/L is preheated to 90°C, added to 250ml of bottom water at 90°C in 15min, heated and stirred while adding titanium solution, and heated to the first time in 20min.
  • Boiling keep boiling, until the system steel is gray, stop heating and reduce the stirring speed for about 25min, then continue heating and stirring to the second boiling, maintain the system micro-boiling state for 25min ; slowly add dilution water to the system, and maintain the whole system
  • the microboiling state was completed until the end of the hydrolysis, and the hydrolysis reaction time was 3.0 h to obtain a hydrolyzate.
  • the hydrolyzed material is subjected to secondary suction washing, Ti 3+ reduction bleaching, calcination seeding, secondary suction washing, addition of KP Al salt treatment agent, temperature-programmed muffle furnace calcination, crucible grinding, inorganic coating, etc. Process, get the product.
  • the suction filtration washing is a laboratory vacuum suction washing, and the vacuum degree 0.1 MPa Ti 3+ reduction bleaching is prepared according to the conventional process in the art and using aluminum powder to reduce the titanyl sulfate.
  • the Ti 3+ reducing agent is used, and the calcined seeds are all prepared by an alkali solution method, and the rutile type Ti0 2 conversion rate is 98%.
  • Example 2 1500ml concentrated 195g / L concentrated titanium liquid preheated to 93 ° C, added to 300ml of bottom water at 93 °C in 18 min, while adding titanium liquid heating and stirring, heating the system to the second in 25 min Once boiled, keep it slightly boiling until the system steel is gray, stop heating and reduce the stirring speed for about 30min, then continue heating and stirring until the second boiling, maintain the system micro-boiling state for 30min ; slowly add dilution water to the system and maintain The whole system was slightly boiled until the end of the hydrolysis, and the hydrolysis reaction time was 3.0 h to obtain a hydrolyzate.
  • the hydrolyzate is subjected to one suction filtration washing, Ti 3+ reduction bleaching, calcination seeding, secondary suction washing, addition of K, P, Al salt treatment agent, temperature-programmed muffle furnace calcination, hydrazine in the same manner as in the examples.
  • the inorganic coating is post-treated to obtain the product.
  • ZZZ L concentrated titanium liquid is preheated to 96 ° C, added to 330 ml of bottom water at 98 ° C in 25 min, heated while stirring with titanium solution, the system is in 23 min Heat to the first boiling, keep the boiling, until the system steel gray, stop heating and reduce the stirring speed for about 35min, then continue heating and stirring to the second boiling, maintain the system micro-boiling state for 35min ; slowly add dilution water to the system And maintaining the micro-boiling state of the whole system until the end of the hydrolysis, the hydrolysis reaction time is 3.5 h, and the hydrolyzate is obtained.
  • the hydrolysis material is subjected to one suction filtration washing, Ti 3+ reduction bleaching, adding calcined seed crystal, secondary suction washing, adding K, P, Al salt treatment agent, temperature-programmed muffle furnace calcination, crucible grinding, inorganic package After treatment with a film or the like, a product is obtained.
  • Example 4 large production test
  • the hydrolyzed material is subjected to primary pressure filtration washing, Ti 3+ reduction bleaching, addition of calcined seed crystals, secondary pressure filtration washing, addition of K, P, Al salt treatment agent, rotary kiln calcination, Raymond grinding, inorganic coating and the like. , get the product.
  • the filter press washing is the filter press washing of the shop press filter
  • the pressure of the press filter is 0.4 ⁇ 0.5 MPa
  • the Ti 3+ reduction bleaching is performed according to the conventional process in the art and the aluminum sulfate is used to reduce the sulfuric acid.
  • the hydrolyzed material is subjected to a primary pressure filtration washing, Ti 3+ reduction bleaching, addition of calcined seed crystals, secondary pressure filtration washing, addition of K, P, Al salt treatment agent, rotary kiln calcination, Raymond grinding, inorganic coating, etc. Process, get the product.
  • Table 1 is a comparison of the product quality of the rutile titanium dioxide obtained by the method of the embodiment of the present invention and the method of the comparative example and the same post-treatment. The results are as follows:
  • the hydrolysis rate does not change much, mainly due to the difference in the washing effect of the hydrolyzate after hydrolysis, especially in the two large productions (Example 4 and Comparative Example).
  • the content of Fe decreased obviously after pressure filtration, and the content of Fe after secondary pressure filtration was lower.
  • the brightness and whiteness of the product quality were greatly improved, and the brightness and whiteness were higher than those of the original high concentration titanium solution.
  • the method of the invention is simple and easy to implement, has no change to the existing process flow, only reduces the concentration of titanium liquid, reduces the amount of bottom water, can improve washing, saves concentrated steam, reduces cost, improves quality, has strong feasibility, and has wide application prospect.

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Abstract

一种低浓度钛液制备高亮度金红石钛白粉的水解方法,包括按体积比1:(4.5〜6)将底水与浓度为190〜215g/L的钛液预热,混合,将混合体系加热至沸腾,并维持微沸状态,当体系成钢灰色时,停蒸汽,降一段时间,继续加热和搅泮到第二次沸腾,维持体系微沸状态一段时间,再向体系缓慢补加稀释水,并维持整个体系微沸状态直到水解结束;上述方法能够降低钛液的浓度,减少底水量,节约浓缩蒸汽,改善洗涤效果,提高产品质量,降低生产成本。

Description

低浓度钛液制备高亮度金红石钛白粉的水解方法 ¾ ^领域
本发明涉及一种硫酸法生产钛白粉的生产工艺中低浓度钛液自生晶种水解 制备高亮度金红石钛白粉的水解方法。
背景技术
在硫酸法生产钛白粉的生产工艺中,决定钛白产品质量的主要因素是水解工 艺的选择, 水解作用的优劣不仅影响工业生产的经济性, 而且对最终产品的质量 也有极大关系。硫酸法金红石钛白粉与氯化法产品相比, 在白度、 亮度等性质存 土 , .因是硫酸法钛白粉中具有较多的有色杂质,并且在粒度尺寸、 分布及形貌上也存在较大的差距。有采用硫酸法制备高亮度的钛白粉方法, 如专 利 CN101851435, 但都是采用繁多的后处理工序, 增加工序和成本。
一般自身晶种稀释水解法, 因为底水量大, 一般在 1 : (3.5-4), 要求很高的 钛液浓度, 很多专利中都要求在 220g/L以上(甚至 250-260 g L ), 这样对整个钛 白生产过程中,浓缩岗位成了生产瓶颈之一,特别是温度低的冬天,浓缩速度慢, 蒸汽耗量高, 钛液的产量受限, 最后影响整个产能。
因此本发明本着优化水解方案,不增加工序,不增添设备,适当降低底水量, 降低钛液浓度, 改善水解料的洗涤性, 改善偏钛酸中杂质含量, 改善产品的粒子 形貌,达到改善白度、亮度等颜料性能的目的,同时可达到降低生产成本的目的。 发明内容
本发明的目的在于克服上述缺陷,提供一种低浓度钛液制备高亮度金红石钛 白粉的水解方法, 在现有的自生晶种水解工艺技术基础上, 降低钛液浓度, 减少 底水量的一种新的水解方法,节约浓缩蒸汽,降低生产成本,同时提高产品质量。
本发明的目的是这样实现的:
一种低浓度钛液制备高亮度金红石钛白粉的水解方法, 包括如下步骤: a、 向水 解锅内加入预热的底水; b、 取经过预热的钛液并缓慢加入到所述底水中, c、加 热步骤 b所得物料至沸腾,并保持微沸状态至该物料变为钢灰色,然后停止加热 并降低搅拌速度; d、 再次升温物料至微沸, 并保持微沸状态 20〜35min; e、于 微沸状态下向物料内加入稀释水, 确保物料中的总钛浓度为 160〜170g/L, 并继 续保持微沸状态至水解结束; 其中, 步骤 b所述钛液浓度的总钛浓度为 190〜 215g/L; 底水与钛液的体积比 1 : (4.5〜6)。
水解方程式: Ti(S04)2+H20→TiOS04+H2S04
TiOS04+2H20→H2Ti03 \ +H2S04
本工艺中, 底水及钛液均各自预热到 90〜98°C, 步骤 b所述钛液可以是采 用钛精矿酸解、 沉降结晶的钛液, 也可以是采用高钛渣酸解、 沉降过滤的钛液, 钛液中 Fe/Ti02的质量比控制在 0.25〜0.35, 其预热一般采用蒸汽加热的方式; 预热钛液在 15〜25min内全部加入底水中, 步骤 c中物料是在 20〜25 min内加 热至沸腾; 而步骤 e中钛液稀释浓度可参照现有钛液水解工艺的参数。
因为钛液水解时, 钛液的浓度对产品质量影响不是主要因素, 而是决定于钛 初始浓度却受到钛液浓度与底水量的控制。相同钛液浓度下 随底水量增加而降低; 相同底水量下随钛液浓度提高而提高。底水量多少决定水 解晶种数量、质量,决定偏钛酸的质量好坏,并最终决定产品质量。一般底水多, 形成结晶中心数量多, 水解速度快, 水解率高, 水合二氧化钛的一次原级粒子较 细, 由于细粒子的表面自由能较大, 容易絮凝成大颗粒而沉降下来, 洗涤时速度 快, 时间短, 但洗涤时间太短容易形成洗涤短路反而不利于铁等杂质的洗涤,影 响白度、 亮度和消色力。 如果钛液浓度过低, 保证水解初始浓度, 则添加的底水 量就太少, 那么结晶中心数量少, 水解速度慢, 水合二氧化钛的一次原级粒子较 粗, 不利于水解料絮凝, 影响洗涤; 水解率低、 收率低; 且最终产品白度、 亮度 等性能差。因此选择适宜的浓度和底水量,控制适宜的晶种量,适宜的水解速率, 和适宜的水合二氧化钛的一次原级粒子, 有助于改善洗涤效果, 提高产品质量。
本工艺控制钛液浓度、 钛液用量及底水用量比, 能够起到优化水解工艺, 改 善洗涤效果、 提高产品质量的效果。
另一方面, 众所周知在传统自生晶种法钛白粉生产过程中, 浓缩是其瓶颈之 一, 因为钛液浓度要求越高, 浓缩压力越大, 一般要求钛液浓度在 220g /L以上, 平均蒸发 It水即消耗 It蒸汽,如果将钛液浓度降低为 205g/L,每生产 It (折 Ti02) 钛液可节约蒸汽 0.38吨,加之少加的底水所耗加热蒸汽,可实现 50元 /吨的成本 节约。 本工艺降低钛液浓度, 减少底水量用量, 保证水解效果的同时, 使过程中 无需再有蒸汽浓缩等工艺环节, 节约成本。
优选的, 底水与钛液体积比为 1 : ( 5〜5.5 )。 底水量是影响水解料洗涤效果的 最主要因素, 底水量主要影响晶种的数量, 晶种多, 结晶中心数量多, 水合二氧 化钛的一次原级粒子较细, 由于细粒子的表面自由能较大, 容易絮凝成大颗粒而 沉降下来, 洗涤时速度快, 时间短, 但洗涤时间太短容易形成洗涤短路又不利于 铁的洗涤, 本工艺中, 最佳的底水量 1 : ( 5 5.5 )。
本发明的技术效果:
本发明所述方法是在现有钛液水解工艺上进行的改进,在不增加任何工序, 不增 添任何设备投资情况下, 降低浓缩钛液浓度, 减少底水量用量, 却能改善水解料 的洗涤性, 改善偏钛酸中杂质含量, 改善产品的粒子形貌, 达到改善白度、 亮度 等颜料性能的目的, 提高了产品质量和产能, 大大降低生产成本, 在产业应用中 具体实 式
下面结合实施例对本发明的具体实施方式做进一步的描述, 而不是以任何方 式来限制本发明。
实施例 1
1500ml浓度为 190g/L的浓钛液预热到 90°C, 在 15min内加入到 250ml温度为 90°C的底水中, 边加钛液边加热搅拌, 在 20min将该体系加热到第一次沸腾,保 持微沸, 直至体系钢灰色, 停止加热和降低搅拌速度约 25min, 后继续加热和搅 拌到第二次沸腾, 维持体系微沸状态 25min; 向体系缓慢补加稀释水, 并维持整 个体系微沸状态直到水解结束, 水解反应时间为 3.0h, 得水解料。将水解料进行 次抽滤洗涤、 Ti3+还原漂白、 加煅烧晶种、 二次抽滤洗、 添加 K P Al盐处 理剂、 程序升温马弗炉煅烧、 擂溃机研磨、 无机包膜等后处理, 得到产品。 本实 施例、 实施例 1和实施例 2中, 抽滤洗涤均为实验室真空抽滤洗涤, 真空度 0.1MPa Ti3+还原漂白均按本领域常规工艺并采用铝粉还原硫酸氧钛制备的 Ti3+ 还原剂进行, 煅烧晶种均为采用碱溶法制备得到的, 金红石型 Ti02 转化率 R 98%。 (碱溶法为: 用 42%碱与漂白干净的偏钛酸 (TiO2 300g/L ) 在高温下煮 沸 3 4h, 生成钛酸钠, 冷却后, 用水洗净游离碱和硫酸根, 再用法盐酸中和至 PH=3.5, 生成正钛酸, 继续加入盐酸, 在 100 110°C煮沸 2h,急冷 40°C, 即得 晶种)
实施例 2 1500ml浓度为 195g/L的浓钛液预热到 93°C, 在 18 min内加入到 300ml温度为 93 °C的底水中, 边加钛液边加热搅拌, 在 25 min将该体系加热到第一次沸腾, 保持微沸, 直至体系钢灰色, 停止加热和降低搅拌速度约 30min, 后继续加热和 搅拌到第二次沸腾, 维持体系微沸状态 30min; 向体系缓慢补加稀释水, 并维持 整个体系微沸状态直到水解结束, 水解反应时间为 3.0h, 得水解料。采用与实施 例相同步骤将水解料进行一次抽滤洗涤、 Ti3+还原漂白、 加煅烧晶种、 二次抽滤 洗、 添加 K、 P、 Al盐处理剂、 程序升温马弗炉煅烧、 擂溃机研磨、 无机包膜等 后处理, 得到产品。
实施例 3
::: ^^;'. ZZZ L的浓钛液预热到 96°C, 在 25 min内加入到 330ml温度为 98°C的底水中, 边加钛液边加热搅拌, 在 23min将该体系加热到第一次沸腾,保 持微沸, 直至体系钢灰色, 停止加热和降低搅拌速度约 35min, 后继续加热和搅 拌到第二次沸腾, 维持体系微沸状态 35min; 向体系缓慢补加稀释水, 并维持整 个体系微沸状态直到水解结束, 水解反应时间为 3.5h, 得水解料。将水解料进行 一次抽滤洗涤、 Ti3+还原漂白、 加煅烧晶种、 二次抽滤洗、 添加 K、 P、 Al盐处 理剂、 程序升温马弗炉煅烧、 擂溃机研磨、 无机包膜等后处理, 得到产品。 实施例 4 (大生产试验)
65M3浓度为 205g/L的浓钛液预热到 98°C, 在 25 min内加入到 14 M3温度为 95 °C的底水中, 边加钛液边加热搅拌, 在 25 min将该体系加热到第一次沸腾, 保 持微沸, 直至体系钢灰色, 停止加热和降低搅拌速度约 35min, 后继续加热和搅 拌到第二次沸腾, 维持体系微沸状态 30min; 向体系缓慢补加稀释水, 并维持整 个体系微沸状态直到水解结束, 水解反应时间为 3.5h, 得水解料。将水解料一次 压滤洗涤、 Ti3+还原漂白、 加煅烧晶种、 二次压滤洗、 添加 K、 P、 Al盐处理剂、 转窑煅烧、 雷蒙磨研磨、 无机包膜等后处理, 得到产品。 本实例及以下对比实施 例中, 压滤洗涤均为车间压滤机压滤洗涤, 压滤的压力为 0.4〜0.5MPa、 Ti3+还原 漂白均按本领域常规工艺并采用铝粉还原硫酸氧钛制备的 Ti3+还原剂,煅烧晶种
(同实例 1 ), 金红石型 Ti02转化率 R 98%。
对比实例 (大生产)
65M3浓度为 240g/L的浓钛液预热到 98°C, 在 25 min内加入到 17 M3温度为 98 °C的底水中, 边加钛液边加热搅拌, 在 25 min将该体系加热到第一次沸腾, 保 持微沸, 直至体系钢灰色, 停止加热和降低搅拌速度约 35min, 后继续加热和搅 拌到第二次沸腾, 维持体系微沸状态 35min; 向体系缓慢补加稀释水, 并维持整 个体系微沸状态直到水解结束, 水解反应时间为 3.5h, 得水解料。将水解料进行 一次压滤洗涤、 Ti3+还原漂白、 加煅烧晶种、 二次压滤洗、 添加 K、 P、 Al盐处 理剂、 转窑煅烧、 雷蒙磨研磨、 无机包膜等后处理, 得到产品。
表 1为采用本发明实施例的方法和对比实施例的方法水解和相同后处理得到 的金红石钛白粉的产品质量方面的对比, 结果如下:
表 1
Figure imgf000006_0001
由表 1 可见, 采用本发明的方法后, 水解率变化不大, 主要是水解后水解 料洗涤效果差异, 特别是大生产两种 (实施例 4和对比例) 水解料的差异很大, 一次压滤洗涤后 Fe含量降低明显, 二次压滤洗涤后 Fe含量也更低, 对产品质量 的亮度、 白度提高很大, 其亮度和白度均高于原高浓度钛液水解的产品质量。 本发明的方法简单易行, 对现有工艺流程没有改变, 仅仅降低钛液浓度, 减少底 水量, 可改善洗涤, 节约浓缩蒸汽, 降低成本, 提高质量, 可行性强, 应用前景 广。
最后需要说明, 以上实施例仅用于说明本发明的技术方案而非限制,尽管参 照较佳实施例对本发明的技术方案进行了详细说明, 本领域技术人员应当理解, 可以对本发明的技术方案进行修改或者等同替换, 而不脱离本发明的宗旨和范 围, 其均应涵盖在本发明的保护范围当中。

Claims

1. 一种低浓度钛液制备高亮度金红石钛白粉的水解方法, 包括如下步骤: a、向 水解锅内加入预热的底水; b、 取经过预热的钛液并缓慢加入到所述底水中, c、 加热步骤 b所得物料至沸腾, 并保持微沸状态至该物料变为钢灰色, 然后停止加 热并降低搅拌速度; d、 再次升温物料至微沸, 并保持微沸状态 20〜35min; e、 于微沸状态下向物料内加入稀释水, 并继续保持微沸状态至水解结束; 其特征在 于: 步骤 b所述钛液浓度的总钛浓度为 190〜215g/L; 底水与钛液的体积比为 1 : ( 4. 5-6 )。
2.根据权利要求 1所述的水解方法, 其特征在于: 底水与钛液体积比为 1 : ( 5- 5· 5 )。
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104030346A (zh) * 2014-06-27 2014-09-10 安徽金星钛白(集团)有限公司 一种高白度金红石型钛白粉的制备方法
CN112108137A (zh) * 2020-10-19 2020-12-22 中国科学院兰州化学物理研究所 一种均匀制备凹凸棒石-二氧化钛复合材料的方法

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102627319B (zh) * 2012-04-24 2014-10-08 攀枝花学院 采用低浓度钛液水解生产颜料钛白的方法
CN103183377B (zh) * 2013-03-04 2015-02-04 广西金茂钛业有限公司 硫酸法钛白粉工艺中低浓度自生晶种水解方法
CN105329941B (zh) * 2015-11-18 2017-03-15 攀钢集团攀枝花钢铁研究院有限公司 减少钛白粉中小颗粒钛白的方法
CN105905941B (zh) * 2016-06-15 2017-11-14 四川龙蟒钛业股份有限公司 一种硫酸法钛白粉工艺中低浓度水解方法
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003033660A (ja) * 2001-07-19 2003-02-04 Akio Komatsu 水和ルチル型二酸化チタン光触媒及び水和処理方法
CN1559913A (zh) * 2004-02-13 2005-01-05 四川龙蟒集团有限责任公司 一种金红石型钛白粉的制备方法
CN101088606A (zh) * 2006-06-12 2007-12-19 中国科学院理化技术研究所 纳米二氧化钛/二氧化硅复合光催化溶胶的制备方法及透明光催化膜
CN101284680A (zh) * 2008-05-05 2008-10-15 攀钢集团攀枝花钢铁研究院有限公司 一种制备钛白的水解方法

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101555038B (zh) * 2009-04-28 2010-12-08 攀钢集团攀枝花钢铁研究院有限公司 通过水解制备钛白粉的方法
CN102145295B (zh) * 2011-01-27 2012-10-17 攀枝花学院 制备掺杂多孔二氧化钛的方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003033660A (ja) * 2001-07-19 2003-02-04 Akio Komatsu 水和ルチル型二酸化チタン光触媒及び水和処理方法
CN1559913A (zh) * 2004-02-13 2005-01-05 四川龙蟒集团有限责任公司 一种金红石型钛白粉的制备方法
CN101088606A (zh) * 2006-06-12 2007-12-19 中国科学院理化技术研究所 纳米二氧化钛/二氧化硅复合光催化溶胶的制备方法及透明光催化膜
CN101284680A (zh) * 2008-05-05 2008-10-15 攀钢集团攀枝花钢铁研究院有限公司 一种制备钛白的水解方法

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104030346A (zh) * 2014-06-27 2014-09-10 安徽金星钛白(集团)有限公司 一种高白度金红石型钛白粉的制备方法
CN112108137A (zh) * 2020-10-19 2020-12-22 中国科学院兰州化学物理研究所 一种均匀制备凹凸棒石-二氧化钛复合材料的方法

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