WO2013020430A1 - Procédé de préparation d'un produit rutile à haute dispersion - Google Patents

Procédé de préparation d'un produit rutile à haute dispersion Download PDF

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Publication number
WO2013020430A1
WO2013020430A1 PCT/CN2012/078205 CN2012078205W WO2013020430A1 WO 2013020430 A1 WO2013020430 A1 WO 2013020430A1 CN 2012078205 W CN2012078205 W CN 2012078205W WO 2013020430 A1 WO2013020430 A1 WO 2013020430A1
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WIPO (PCT)
Prior art keywords
rutile
titanium dioxide
water
product
crude
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PCT/CN2012/078205
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English (en)
Chinese (zh)
Inventor
代堂军
蔡平雄
常键
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 WO2013020430A1 publication Critical patent/WO2013020430A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
    • C01G23/0532—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing sulfate-containing salts
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • C—CHEMISTRY; METALLURGY
    • 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
    • C09C1/36—Compounds of titanium
    • C—CHEMISTRY; METALLURGY
    • 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
    • C09C1/36—Compounds of titanium
    • C09C1/3607—Titanium dioxide
    • C09C1/3653—Treatment with inorganic compounds
    • C—CHEMISTRY; METALLURGY
    • 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
    • C09C1/36—Compounds of titanium
    • C09C1/3607—Titanium dioxide
    • C09C1/3669—Treatment with low-molecular organic compounds

Definitions

  • the invention relates to a preparation method of rutile type titanium dioxide, in particular to a preparation method of rutile with specific high dispersibility.
  • Titanium dioxide is one of the most important inorganic pigments and chemical raw materials. Pigment grade titanium dioxide is mainly used in coatings, paper, plastics, rubber, latex paints, printing inks, chemical fiber and other industries. Non-pigment grade titanium dioxide is mainly used in enamel, capacitors and welding electrodes.
  • the production method of titanium dioxide is generally classified into a sulfuric acid method and a chlorine method.
  • the sulfuric acid method is a common traditional production method, and the steps generally include: the acid hydrolysis reaction of titanium iron powder with concentrated sulfuric acid to produce titanium sulfate sulfate, sedimentation, crystallization, hydrolysis to form meta-antimonic acid, and the addition of metatitanic acid Bleaching, second washing, salt treatment, calcination to obtain crude rutile titanium dioxide, wet titanium dioxide added to the dispersing agent, wet grinding to obtain rutile titanium dioxide slurry, sanding, and then coating the film and gas powder to obtain the product.
  • a plurality of metal ions are generally added to the metatitanic acid as a salt treatment agent before calcination, and these metal ions include potassium and sodium.
  • These metal ions include potassium and sodium.
  • the purpose of adding potassium and phosphorus during the calcination of metatitanic acid is to obtain a softer crude rutile titanium dioxide for subsequent grinding; the addition of aluminum is to improve the weatherability and pigment properties of the pigment; the addition of zinc, lithium and magnesium is mainly
  • the calcination strength is lowered.
  • a certain amount of calcined seed crystals are added to the metatitanic acid to be calcined to lower the calcination temperature to obtain pigment particles having a suitable particle diameter.
  • the salt treatment agent is converted into a sulfate or an oxide, and the content of the water-soluble salt is generally
  • the S0 3 meter is based on 0.30-1.00% of the total rutile type titanium dioxide, and the dispersion effect of the cerium oxide slurry cannot be improved even under the action of a large amount of dispersing agent, and even the grinding cannot be continued, so that the water dispersibility of the pigment particles is lowered, and further Affects the quality of the grinding and the dispersion of the rutile finished product.
  • the dispersibility of the rutile finished product is the most important quality index of titanium dioxide. Good dispersibility is of great significance for improving the pigment performance of titanium dioxide and reducing the grinding time.
  • the methods currently used are to reduce the calcination strength of metatitanic acid, to extend the sanding time, and to make a reasonable replacement page (Article 26) Membrane treatment and improvement of gas powder strength, etc.
  • these methods have great limitations.
  • reducing the calcination strength of metatitanic acid will reduce the weather resistance of the product; prolonging the sanding time will pollute the raw materials and reduce the brightness of the product; the effect of the coating on the dispersibility of the finished titanium dioxide is not obvious;
  • the method of improving the dispersibility of the finished product has high energy consumption and is not cost-effective. There has been no research to improve the dispersibility of rutile products by improving the pre-crushing effect of titanium dioxide.
  • An object of the present invention is to provide a method for significantly increasing the rutile dispersibility in view of the above problems.
  • a preparation method of a highly dispersed rutile product which is produced by a sulfuric acid method, and includes the following steps in sequence: an acid hydrolysis reaction of titanium concentrate with concentrated sulfuric acid to produce titanium sulfate, and then hydrolyzed to form a partial Titanic acid, salt treatment, calcination to obtain crude rutile titanium dioxide, titanium dioxide crude added to the dispersant, wet grinding to obtain rutile titanium dioxide slurry, sand, coated and gas powder to obtain titanium dioxide finished product, obtained by calcination
  • the crude rutile titanium dioxide is washed with water to reduce the content of the water-soluble salt therein, and then the water-washed rutile-type titanium dioxide is further added to a dispersing agent for wet grinding.
  • the crude rutile-type titanium dioxide obtained by calcination is washed with water to reduce the content of the water-soluble salt therein to 0.25% or less based on the mass of the washed rutile-type titanium dioxide based on S0 3 .
  • the experimental results show that the lower the water-soluble salt content, the better the dispersibility of the rutile product obtained under the same conditions.
  • the dispersing agent is at least one of sodium hydroxide, sodium silicate, sodium hexametaphosphate, sodium polycarboxylate, monoethanolamine, and monoisopropanolamine.
  • the dispersant is added in an amount of from 0.05 to 0.60% based on the mass of the total titanium dioxide in the rutile-type titanium dioxide slurry.
  • the water washing method is a method in which a crude rutile-type titanium dioxide obtained by calcination is mixed with water, stirred, allowed to stand and decanted, and the above operation is repeated as necessary.
  • the inventors of the present application have found through a large number of studies that if the crude rutile titanium dioxide is not subjected to a water washing process and the amount of the dispersant is 0.05-3.00% based on the mass of the total titanium dioxide in the rutile-type titanium dioxide slurry, the wet milling feed concentration is controlled to the highest. in the titanium dioxide meter 400-700g / L; when the rutile titania after washing process, the water-soluble salts of titanium dioxide in the S0 3 content of the total count of less than 0.25% titanium dioxide based on the amount of dispersant may be only 0.20%
  • the wet mill feed concentration is between 800 and 1400 g/L in terms of titanium dioxide.
  • the crude rutile is washed away with most of the coarse salt to increase the wet grinding concentration.
  • Washed rutile crude product may take a wide variety of devices, the easiest way is to mix titanium dioxide and water, stirring, settling and decanting operation is repeated until the number of the water-soluble salt content of titanium dioxide so 3 based on the total titanium oxide is less than 0.25% .
  • the beneficial effects of the present invention are as follows: the rutile product prepared by the method of the invention has an alkyd resin system having a 20 degree gloss of 120 degrees or more, and the crude rutile product is not washed with water, and then the same post-treatment method is adopted.
  • the prepared rutile product has an alkyd resin system with a dispersibility of 20 degrees gloss of up to 100, and the amount of dispersant in the wet grinding process is greatly reduced, which not only saves cost but also greatly improves product dispersion performance.
  • the bleached qualified metatitanic acid is phosphoric acid (0.20% by mass of phosphorus pentoxide), potassium sulfate (0.30% by mass of potassium oxide) and aluminum sulfate (0.33 by mass of aluminum oxide) %)
  • phosphoric acid 0.20% by mass of phosphorus pentoxide
  • potassium sulfate 0.30% by mass of potassium oxide
  • aluminum sulfate (0.33 by mass of aluminum oxide) %)
  • the obtained slurry was sanded, and the coated film was processed to obtain the rutile finished product A.
  • the 20 degree gloss data of A is shown in Table 1.
  • Example 1 The calcined product of Example 1 was added to a dispersant sodium silicate solution at a mass of 0.20% of total titanium dioxide, and water was beaten to a titanium dioxide content of 1000 g/L, and the obtained slurry was subjected to a ball mill grinding, sanding, and coating in Example 1. After the film is processed, the rutile finished product B is obtained, and the 20-degree gloss data of B is shown in Table 1.
  • Example 1 The calcined product of Example 1 was taken, and the salt content was reduced to 0.50% by a water washing operation, and the dispersant sodium silicate solution was added to 0.20% of the total titanium dioxide mass, and water was beaten to a titanium oxide content of 1000 g/L, and the obtained slurry was implemented.
  • the ball mill was used for grinding, sanding, and coating to obtain the rutile finished product C, and the 20 degree gloss data of C is shown in Table 1.
  • Example 1 The calcined product of Example 1 was taken, and the salt content was reduced to 0.40% by a water washing operation, and the dispersant sodium silicate solution was added to 0.20% of the total titanium dioxide mass, and water was beaten to a titanium oxide content of 1000 g/L, and the obtained slurry was subjected to implementation.
  • the ball mill was used for grinding, sanding, and the coating was awaiting treatment to obtain the rutile finished product D.
  • the 20 degree gloss data of D is shown in Table 1.
  • Example 1 The calcined product of Example 1 was taken, and the salt content was reduced to 0.30% by a water washing operation, and the dispersant sodium silicate solution was added at 0.20% of the total titanium dioxide mass, and water was beaten to a titanium oxide content of 1000 g/L, and the obtained slurry was subjected to a slurry.
  • the ball mill was used for grinding, sanding, and the coating was awaiting treatment to obtain the rutile finished product E.
  • the 20 degree gloss data of E is shown in Table 1.
  • Example 1 The calcined product of Example 1 was taken, and the salt content was reduced to 0.25% by a water washing operation, and the dispersant sodium silicate solution was added at 0.20% of the total titanium dioxide mass, and water was beaten to a titanium oxide content of 1000 g/L, and the obtained slurry was subjected to a slurry.
  • the ball mill was used for grinding, sanding, and the coating was awaiting treatment to obtain the rutile finished product F.
  • the 20 degree gloss data of F is shown in Table 1.
  • Example 1 The calcined product of Example 1 was taken, and the salt content was reduced to 0.20% by a water washing operation, and the dispersant sodium silicate solution was added to 0.20% of the total titanium dioxide mass, and the slurry was added with water to a titanium oxide content of 1000 g/L, and the obtained slurry was implemented.
  • the ball mill was used for grinding, sanding, and the coating was awaiting treatment to obtain the rutile finished product G.
  • the 20 degree gloss data of G is shown in Table 1.
  • Example 1 The calcined product of Example 1 was taken, and the salt content was reduced to 0.10% by a water washing operation, and the dispersant sodium silicate solution was added to the total titanium dioxide mass 0.05%, and the water was beaten to a titanium dioxide content of 1000 g/L, and the obtained slurry was carried out.
  • the ball mill was used for grinding, sanding, and the coating was awaiting treatment to obtain rutile.
  • Example 1 The calcined product of Example 1 was taken, and the salt content was reduced to 0.10% by a water washing operation, and the dispersant sodium silicate solution was added to 0.20% of the total titanium dioxide mass, and water was beaten to a titanium dioxide content of 1000 g/L, and the obtained slurry was subjected to a slurry.
  • Example 1 the 20-degree gloss data of the rutile finished product I, I obtained by grinding with a ball mill, sanding, and coating waiting for treatment is shown in Table 1.
  • the dispersion of titanium dioxide finished products is still very poor (Comparative Examples 1 and 2); Moreover, the smaller the rutile crude salt content after washing under the same conditions, the better the dispersibility; at the same time, compared with the water-washed, washed After that, the amount of dispersing agent used in rutile crude wet grinding is greatly reduced, and the obtained rutile finished product has higher dispersibility, and the dispersing agent is saved, and a higher dispersible rutile product can be obtained.

Abstract

L'invention concerne un procédé de préparation d'un produit rutile à haute dispersion fabriqué par un procédé à l'acide sulfurique, le procédé comprenant les étapes de : réaction d'acidolyse, hydrolyse pour générer de l'acide métatitanique, traitement par un sel, calcination, broyage par voie humide, puis broyage au broyeur à sable, enrobage et broyage par soufflage d'air, de façon à obtenir du dioxyde de titane fini ; lavage du produit brut dioxyde de titane rutile résultant de la calcination avec de l'eau pour réduire la teneur en sels solubles dans l'eau dans celui-ci, puis addition d'un agent dispersant au dioxyde de titane rutile lavé et broyage par voie humide. Le produit rutile préparé par le procédé a un système de résine alkyde ayant une dispersité de 20° et un brillant allant jusqu'à plus de 120. Le procédé utilise une quantité réduite de l'agent dispersant dans le broyage par voie humide, économise les coûts et améliore la propriété de dispersion du produit.
PCT/CN2012/078205 2011-08-11 2012-07-05 Procédé de préparation d'un produit rutile à haute dispersion WO2013020430A1 (fr)

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CN201110229324.9 2011-08-11
CN 201110229324 CN102391689B (zh) 2011-08-11 2011-08-11 一种高分散金红石产品的制备方法

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CN103265069B (zh) * 2013-05-14 2015-09-30 中国科学院过程工程研究所 一种制备金红石型二氧化钛的方法
CN104119703B (zh) * 2014-07-22 2015-11-18 四川龙蟒钛业股份有限公司 一种高光泽金红石型钛白粉的制备方法
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CN107057407A (zh) * 2016-12-23 2017-08-18 宁波新福钛白粉有限公司 一种水性漆用二氧化钛颜料的制备方法
CN106698508A (zh) * 2017-01-10 2017-05-24 四川龙蟒钛业股份有限公司 钛白粉基料的生产方法
CN108083331B (zh) * 2017-12-29 2018-11-23 广东惠云钛业股份有限公司 一种金红石型二氧化钛超细粉的制备方法
CN109052716B (zh) * 2018-08-29 2020-09-08 北部湾大学 金红石粗品湿磨工艺，金红石粗品湿磨工艺用碱性水的制备方法
CN109942019B (zh) * 2019-04-23 2021-07-30 广西民族大学 一种加快偏钛酸转化为金红石型二氧化钛的盐处理方法
CN111269588B (zh) * 2020-03-26 2021-09-03 正太新材料科技有限责任公司 一种高着色力的耐热氧化铁黄及其制备方法与应用
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CN115924966A (zh) * 2022-12-12 2023-04-07 龙佰四川钛业有限公司 一种钛白粉盐处理剂回收工艺及钛白粉生产工艺

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