CN106433226A - Titanium dioxide and preparing method thereof - Google Patents

Titanium dioxide and preparing method thereof Download PDF

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Publication number
CN106433226A
CN106433226A CN201610796961.7A CN201610796961A CN106433226A CN 106433226 A CN106433226 A CN 106433226A CN 201610796961 A CN201610796961 A CN 201610796961A CN 106433226 A CN106433226 A CN 106433226A
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value
titanium dioxide
slurry
preparation
mass concentration
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Inventor
李后明
陈寿华
何彬
罗春丽
杨家全
伍春波
周兵
袁晓艳
钟秀琴
雷刚
包天贵
罗宏
刘洁
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Yunnan Dahutong Titanium Industry Co Ltd
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Yunnan Dahutong Titanium Industry Co Ltd
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    • 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
    • C09C1/3692—Combinations of treatments provided for in groups C09C1/3615 - C09C1/3684
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/02—Ingredients treated with inorganic substances
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C08K9/06—Ingredients treated with organic substances with silicon-containing 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
    • C09C1/3653—Treatment with inorganic compounds
    • C09C1/3661—Coating
    • 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
    • C09C1/3684—Treatment with organo-silicon 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2237—Oxides; Hydroxides of metals of titanium
    • C08K2003/2241—Titanium dioxide

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)

Abstract

The invention provides a titanium dioxide and a preparing method thereof, and relates to the technical field of titanium dioxide. The preparing method comprises the steps of preparing 88-111 parts by mass of titanium dioxide base stock into titanium dioxide slurry, mixing the titanium dioxide slurry with 0.45-0.55 part by mass of zirconium sulfate solution, 0.35-0.45 part by mass of first aluminum sulfate solution, 0.6-0.7 part by mass of sodium metaaluminate solution and 0.04-0.06 part by mass of second aluminum sulfate solution, washing and drying the mixture to obtain an intermediate product, and mixing the intermediate product with 0.06-0.08 part by mass of silane coupling agent to obtain the titanium dioxide. The prepared titanium dioxide has excellent compatibility, processability and mobility in a plastic system and a color master batch system, and meets the requirement of the titanium dioxide for plastics.

Description

A kind of titanium dioxide and preparation method thereof
Technical field
A kind of the present invention relates to field of titanium, and more particularly to titanium dioxide and preparation method thereof.
Background technology
Titanium dioxide is widely used in coating, paint, plastics, papermaking, cosmetics and medical industry.Wherein, coating institute Accounting weight is maximum.Between 30 years, share of the titanium dioxide amount for consuming in total flow is painted, is declined by 62% To 50%, this increases rapider mainly due to amount of titanium in plastic industry and paper industry.
For meeting the market requirement, Producing Titanium Dioxide enterprise attempts to develop the standard titanium being fit for various uses as much as possible In vain.But, this will necessarily produce a problem in the development phase, that is, determine using what performance as leading problem：Be with light It is leading to learn performance, or gloss promotion property is leading, or is leading problem with dispersibility or weatherability, to adapt to respectively answer Use domain requirement.It is a quite meaningful challenge.
In recent years, plastic industry is to the demand of titanium white progressively riseing, but domestic titanium white is " universal titanium white " mostly, I.e.：Any industry can be used, but what industry using effect is all undesirable.For this purpose, targeted different special of exploitation attribute Type titanium dioxide becomes the new tendency of domestic and international titanium dioxide industry development, and the basic object being surface-treated is exactly to improve titanium dioxide The weatherability of titanium pigment, dispersibility and colour retention, this exactly indispensable key property of any excellent pigment.From Different surface conditioning agents, using different processing methods, can produce the titanium dioxide product of different purposes.Therefore surface Processing becomes the major subjects that in various countries' titanium powder industry, technical staff studies for a long period of time and inquires into already, becomes the master of new product development Want means.
Content of the invention
It is an object of the invention to provide a kind of preparation method of titanium dioxide, the preparation method of this titanium dioxide has operation relatively Less and simple to operate the features such as.
Another object of the present invention is to a kind of titanium dioxide is provided, the application in plastic applications is disclosure satisfy that.
The present invention solves its technical problem and employs the following technical solutions to realize.
The present invention proposes a kind of preparation method of titanium dioxide, and which includes：
According to the mass fraction, by 88～111 parts of titanium dioxide base material be prepared into Titanium dioxide slurry and successively with 0.45～ 0.55 part of sulphuric acid zirconium solution, 0.35～0.45 part of the first aluminum sulfate solution, 0.6～0.7 part of sodium aluminate solution and 0.04～0.06 part of the second aluminum sulfate solution mixing, wash and be dried to obtain intermediate product, by intermediate product and 0.06～ 0.08 part of silane coupler is mixed to get titanium dioxide.The preparation method of this titanium dioxide can quickly be prepared and disclosure satisfy that plastic collar The titanium dioxide that applies in domain.
The present invention proposes a kind of titanium dioxide, is obtained according to above-mentioned titanium white powder, preparation method thereof.Obtained titanium dioxide has light Ze Dugao, good dispersion, oil absorption are low, weatherability is high, strong covering power and the features such as blue bottom phase, meet in plastics system In application.
The invention has the beneficial effects as follows：The present invention in the preparation process of titanium dioxide, by inorganic coating and organic bag Film is surface-treated twice, and glossiness height, good dispersion, oil absorption be low, hydrophobicity is good and blue to have obtained titanium dioxide The features such as bottom phase, possess the excellent compatibility, processability and mobility in plastics, color masterbatch system, meet plastics titanium dioxide Requirement.
Description of the drawings
In order to be illustrated more clearly that the technical scheme of the embodiment of the present invention, below by to be used attached needed for embodiment Figure is briefly described, it will be appreciated that the following drawings illustrate only certain embodiments of the present invention, and it is right to be therefore not construed as The restriction of scope, for those of ordinary skill in the art, on the premise of not paying creative work, can also be according to this A little accompanying drawings obtain other related accompanying drawings.
Fig. 1 is the preparation method flow chart of embodiment of the present invention titanium dioxide；
Fig. 2 is the method flow diagram of embodiment of the present invention inorganic coating.
Specific embodiment
Purpose, technical scheme and advantage for making the embodiment of the present invention is clearer, below will be in the embodiment of the present invention Technical scheme be clearly and completely described.In embodiment, unreceipted actual conditions person, builds according to normal condition or manufacturer The condition of view is carried out.Agents useful for same or the unreceipted production firm person of instrument, are and can buy, by commercially available, the conventional product for obtaining Product.
Below titanium dioxide of the embodiment of the present invention and preparation method thereof is specifically described.
Fig. 1 is the flow chart of the preparation method of titanium dioxide provided in an embodiment of the present invention, to the preparation method of titanium dioxide Description is please referred to as follows.
A kind of titanium dioxide and preparation method thereof, which includes：
According to the mass fraction, 88～111 parts of titanium dioxide base material is prepared into Titanium dioxide slurry.Plastics titanium dioxide with logical With differring primarily in that for type titanium dioxide：Plastics titanium dioxide is partial to blue phase, mean diameter little (about 0.22um), and oil absorption is relatively Low.In use, plastics titanium dioxide can not only be with the good compatibility and excellent point in plastic resin Scattered property, will also can provide maximized covering power and brilliant white, and can keep the mechanicalness in plastic application Energy.To sum up, titanium dioxide base material will disclosure satisfy that calcining particle is thin and soft, the tiny and uniform and form and aspect of particle diameter inclined blue phase relatively Require.Titanium dioxide base material is obtained by following methods：From metatitanic acid obtained in conventional method, before calcination, forge according to rutile Crystal seed is burnt (with TiO2Meter) with the mass ratio of metatitanic acid be：100th, according to potassium carbonate (with K2CO3Meter) with the mass ratio of metatitanic acid For 0.7：100 and according to phosphoric acid liquid (with contain H3PO4Count for 85% phosphoric acid liquid) with the mass ratio of metatitanic acid be：100 Weigh rutile calcining seeds, potassium carbonate and phosphoric acid liquid to be added in metatitanic acid and mixture is obtained, add mixture to In rotary kiln, rutile content being obtained after rotary kiln calcining and falling kiln product for 97.5～98.5%, falling, kiln product are ground to obtain titanium dioxide Base material.The equipment of grinding can adopt Raymond mill or roll mill.Produce according to the calcining of above-mentioned calcining seeds dosage, salt treatment and rotary kiln Product control rutile conversion ratio, can reduce calcining heat, intensity, reduce transformation of crystal temperature, reduce and avoid particle to burn Knot, hardening, reach the requirement of the titanium dioxide base material for preparing plastics.
Titanium dioxide slurry is obtained by following methods：Above-mentioned titanium dioxide base material is dispersed through, wet grinding, classification obtain particle diameter and be suitable for Titanium dioxide slurry.
Dispersion is be 180～190m/min in the linear velocity of stirring under conditions of by above-mentioned titanium dioxide base material and resistivity >= The desalted water mixing of 200K Ω, during mixing and adds dispersant that divided titanium dioxide dispersion liquid is obtained.Wherein, dispersant Arbitrary proportion at least one or which is multiple in monoisopropanolamine, sodium silicate, sodium hexameta phosphate and carboxylic acid sodium mixes.? During scattered, it is 9～11 by the pH for controlling slurry, TiO can be obtained2The divided titanium dioxide dispersion liquid of concentration >=600g/L.System The divided titanium dioxide dispersion liquid for obtaining possesses relatively low viscosity, is conducive to improving follow-up wet grinding effect.
Wet grinding is that obtained divided titanium dioxide dispersion liquid is added to colloid mill or ceramic grinding after preliminary grinding, is then added to sand The further fine grinding of grinding machine.The TiO that will bond in divided titanium dioxide dispersion liquid2Particle or the TiO of coalescence2Particle is broken up completely, makes titanium dioxide Single TiO is formed in dispersion liquid2Particle, so as to follow-up inorganic coating operation can coating agent is uniform, intactly coat In TiO2Particle surface, improves pigment performance and the using effect of titanium dioxide.
Classification is that separation is wet through vibrosieve, centrifugal clasfficiator or hydrocyclone by the divided titanium dioxide dispersion liquid after wet grinding The coarse granule in divided titanium dioxide dispersion liquid and fine grained after mill, obtains TiO2Granularity be 0.2～0.3 μm of Titanium dioxide slurry. Titanium dioxide slurry with certain particle size distribution is obtained in that by classification, and the requirement of plastics titanium dioxide is prepared with guarantee.Logical Classification is crossed, on the one hand the coarse granule aggregation that isolates can be returned to wet-milling step, re-grind, until it reaches classification mark Standard, improves the utilization rate of raw material, on the other hand, can remove the fine grained mechanical admixtures such as the fine sand that is grated.
Have the characteristics that centralized particle diameter and coarse granule are less by Titanium dioxide slurry obtained in said method.In order to Ensure that follow-up peplos are uniform and complete, in preferred embodiments of the present invention, Titanium dioxide slurry is permissible before inorganic coating Using TiO2Mass concentration be that three wash waters of 10～20g/L are being mixed with above-mentioned Titanium dioxide slurry.Mixing be at 55～60 DEG C At a temperature of stir 60～80min.In other implementations of the present invention, Titanium dioxide slurry can also be adopted before inorganic coating Desalted water dilutes.In Titanium dioxide slurry after dilution, TiO2Mass concentration be 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l,.
Wherein, preferably, the mass concentration of obtained Titanium dioxide slurry is controlled to 280～320g/l, pH value is controlled to 9 ～10.5.In preferred embodiments of the present invention, 0.03～0.036 matter can also be added before inorganic coating in white lead slurry The ammonium dihydrogen phosphate of amount part is (with P2O5Meter), ammonium dihydrogen phosphate is used as a kind of additive, it is possible to increase the pigment performance of titanium dioxide with And the stability of unconverted anatase crystal type.
At a temperature of 55～60 DEG C, the Titanium dioxide slurry after dilution is molten with 0.45～0.55 part of Disulfatozirconic acid. successively Liquid, 0.35～0.45 part of the first aluminum sulfate solution, the of 0.6～0.7 part of sodium aluminate solution and 0.04～0.06 part The mixing of two aluminum sulfate solutions carries out inorganic coating, during the Titanium dioxide slurry after inorganic coating is carried out washing, is dried to obtain Between product, intermediate product is mixed with 0.06～0.08 part of silane coupler to carry out organic coated, obtains titanium dioxide.Wherein, 0.45～0.55 part of sulphuric acid zirconium solution refers to the ZrO in sulphuric acid zirconium solution2Mass parts be 0.45～0.55 part, similarly hereinafter； 0.35～0.45 part of the first aluminum sulfate solution refers to the Al in the first aluminum sulfate solution2O3Mass parts be 0.35～0.45 part, Similarly hereinafter；0.6～0.7 part of sodium aluminate solution refers to Al in sodium aluminate solution2O3Mass parts be 0.6～0.7 part, similarly hereinafter； 0.04～0.06 part of the second aluminum sulfate solution refers to Al in the second aluminum sulfate solution2O3Mass parts be 0.04～0.06 part, under With.
Inorganic coating is by precipitation and to adsorb, in TiO2One or more layers inorganic aqua oxidation is wrapped on particle surface Thing.Above-mentioned sulphuric acid zirconium solution, the first aluminum sulfate solution and the second aluminum sulfate mixture solution of sodium aluminate solution can be autonomous Prepare, it is also possible to buy from market.Fig. 2 is refer to, preparation process all can be carried out in its corresponding preparation vessel, and it is right to be prepared into Corresponding storage tank is entered back into after the solution that answers, and the solution in storage tank enters inorganic coating process tank by allotter, completes Inorganic coating operation.And specifically, it is preferable to control in sulphuric acid zirconium solution：ZrO2Mass concentration be 100～110g/L, H2SO4Matter Amount concentration is 190～210g/L, total iron content≤30ppm.It is preferred that controlling in the first aluminum sulfate solution：Al2O3Mass concentration be 100～110g/L, H2SO4Mass concentration be 270～300g/L, total iron content≤30ppm.It is preferred that control sodium aluminate solution In：Al2O3Mass concentration for 100～110g/L, NaOH mass concentration be 230～245g/L, total iron content≤30ppm.Excellent In the second aluminum sulfate solution of selected control system：Al2O3Mass concentration be 100～110g/L, H2SO4Mass concentration be 190～ 210g/L.Disulfatozirconic acid., aluminum sulfate and sodium metaaluminate are all prepared into solution be conducive to mixing homogeneously with Titanium dioxide slurry, to reach To preferable inorganic coating effect.By inorganic coating, it is possible to increase the weatherability of plastics titanium dioxide and chemical stability.No Machine peplos can block TiO2Particle lattice defect, covers TiO2The photoactivation point of particle surface, can either shield light-catalysed work With the ability of titanium dioxide resistance to chemical attack can also be strengthened.
Specifically, 0.45～0.55 part of sulphuric acid zirconium solution is added in Titanium dioxide slurry with the speed of 12～30L/min, protects At a temperature of holding 55～60 DEG C, continuously stirred 40～50min obtains the first slurry, and the pH value of the first slurry is 1.7～3.0.By 0.35 ～0.45 part of first aluminum sulfate solution is added in the first slurry with the speed of 80～110L/min, at a temperature of being kept for 55～60 DEG C 10～20min of stirring obtains the second slurry, and the pH value of the second slurry is 1.7～2.7.By 0.6～0.7 part of sodium aluminate solution with The speed of 45～60L/min is added in the second slurry, stirs 40～50min and obtain the 3rd slurry at a temperature of being kept for 55～60 DEG C, It is 9.0～9.5 to add NaOH solid in the 3rd slurry and control the pH value of the 3rd slurry.The process of inorganic coating is using first wrapping The step of zirconium, rear alclad, the change of echelon from small to large of the pH value of Titanium dioxide slurry can be realized, is conducive in TiO2Surface shape Uniformly, complete and stable dense film so that the titanium dioxide of preparation has smooth surface, low diffuse-reflectance and high-luster The features such as.In order to adjust the pH value of Titanium dioxide slurry further, 0.04～0.05 part of second aluminum sulfate solution is added to the 3rd In slurry, 20～40min is stirred at a temperature of being kept for 55～60 DEG C and obtains the 4th slurry, then continuously stirred to the 4th slurry 100～ 150min obtains the 5th slurry.Wherein, the pH value of the 5th slurry is 7.0～8.2.By from Disulfatozirconic acid., aluminum sulfate and partially Sodium aluminate is used as inorganic coating agent, it is possible to increase the weatherability of the titanium dioxide of titanium dioxide, glossiness and resistance.
Washing refers to desalted water using resistivity >=200K Ω to things such as inorganic salts for remaining in the 5th slurry Matter is removed and obtains filter cake.Control eluate conductance≤100us/cm, it is qualified that the filter cake for obtaining as is washed.Here need not limit de- The consumption of saline, as long as above-mentioned condition can totally be met i.e. by matter detergent such as the inorganic salts of residual in the 5th slurry Can.By washing, inorganic salts material can be avoided from entering titanium dioxide system, in order to avoid the pigment performance of impact titanium dioxide and use Effect.
Drying is filter cake to be added to removing moisture in flash dryer to obtain intermediate product.Intermediate product be through no The TiO of machine peplos2Powder body.
The organic coated particle surface for being to adsorb by Organic substance surfactants-polar group or be bonded in titanium dioxide, Rely on electric repulsion and space steric effect to improve wettability of the titanium dioxide in various disperse medium, dispersibility and rheology Property.In preferred embodiments of the present invention, in order to preferably realize the effect of organic film, by the step of organic coated and crushing While carrying out：Using pressure be 18～22MPa, temperature be 290～310 DEG C steam to intermediate product and 0.06～0.08 matter The silane coupler of amount part is crushed and is mixed, and silane coupler can be evenly coated at after vaporizing under high pressure and high temperature condition TiO during gas powder2Powder surface, obtains titanium dioxide.In preferred embodiments of the present invention, silane coupler selects octyl group Triethoxysilane, octyltri-ethoxysilane can be provided by octyltriethoxysilane solution.Inorganic coating and organic bag The effect of film is interrelated, further increases the effect of surface treatment.
Titanium dioxide according to obtained in the preparation method of above-mentioned titanium dioxide, with glossiness height, good dispersion, oil absorption Low, weatherability is high, strong covering power and the features such as blue bottom phase, possesses the splendid compatibility and mobility in plastics system, It is a kind of excellent plastics titanium dioxide.
The stirring of the embodiment of the present invention can adopt mechanical agitation, it would however also be possible to employ air stirring, if can realize right The mixed effect that answers.
The present invention in the preparation process of titanium dioxide, by inorganic coating and organic coated be surface-treated twice, make system The titanium dioxide for obtaining has preferable weatherability, dispersibility, mobility and colour retention, meets the requirement of plastics titanium dioxide.
With reference to embodiments the feature and performance of the present invention is described in further detail.
Embodiment 1
At a temperature of 55 DEG C, 25t titanium dioxide base material is mixed with water, be dispersed through, wet grinding, classification are prepared into mass concentration The ammonium dihydrogen phosphate of 0.03t is added for Titanium dioxide slurry that 300g/l, pH value are 8.7 and in Titanium dioxide slurry, is kept stirring for Titanium dioxide slurry 25min.
The Disulfatozirconic acid. of 284.7kg is prepared into 1.125m with sulphuric acid and water reaction3Sulphuric acid zirconium solution, wherein：ZrO2's Mass concentration is 110g/L, H2SO4Mass concentration is 300g/L, and sulphuric acid zirconium solution is at the uniform velocity added titanium white according to 12L/min speed In slurry material and stir 45min and obtain the first slurry.
First aluminum sulfate of 318.5kg is prepared into 0.95m with sulphuric acid and water reaction3The first aluminum sulfate solution, its In：Al2O3Mass concentration be 100g/L, H2SO4Mass concentration be 210g/L, by the first aluminum sulfate solution according to 80L/min Speed is at the uniform velocity added in the first slurry and obtains the second slurry after stirring 15min.
The sodium metaaluminate of 265.9kg is prepared into 1.575m with sodium hydroxide and water reaction3Sodium aluminate solution, its In：Al2O3Mass concentration for 105g/L, NaOH mass concentration be 245g/L, by sodium aluminate solution according to 45L/min speed Degree is at the uniform velocity added in the second slurry and stirs 45min and obtains the 3rd slurry, and now slurry pH value is 9.0.
0.125m is prepared by mixing into the second aluminum sulfate of 41.9kg and sulphuric acid and water3The second aluminum sulfate solution, wherein： Al2O3Mass concentration be 100g/L, H2SO4Mass concentration be 195g/L, the second aluminum sulfate solution is added to the 3rd slurry In and stir 30min and obtain the 4th slurry, the pH of the 4th slurry is 7.8.
4th slurry is continued stirring 120min, inorganic coating terminates to obtain the 5th slurry.5th slurry is used resistance Rate carries out washing for the desalted water of 200K Ω and obtains filter cake.Filter cake drying is obtained middle by product.Using pressure it is 22MPa, temperature is that 310 DEG C of steam is crushed to intermediate product, adds the octyltri-ethoxysilane of 0.2t while crushing Solution obtains titanium dioxide.
Embodiment 2
At a temperature of 55 DEG C, 30t titanium dioxide base material is mixed with water, be dispersed through, wet grinding, classification are prepared into mass concentration The ammonium dihydrogen phosphate of 0.036t is added for Titanium dioxide slurry that 300g/l, pH value are 8.9 and in Titanium dioxide slurry, keeps titanium white Powder slurry agitation 25min.
The Disulfatozirconic acid. of 310.6kg is prepared into 1.35m with sulphuric acid and water reaction3Sulphuric acid zirconium solution, wherein：ZrO2's Mass concentration is 100g/L, H2SO4Mass concentration is 280g/L, and sulphuric acid zirconium solution is at the uniform velocity added titanium white according to 20L/min speed In slurry material and stir 45min and obtain the first slurry.
First aluminum sulfate of 382.2kg is prepared into 1.14m with sulphuric acid and water reaction3The first aluminum sulfate solution, its In：Al2O3Mass concentration be 100g/L, H2SO4Mass concentration be 195g/L, by the first aluminum sulfate solution according to 90L/min Speed is at the uniform velocity added in the first slurry and obtains the second slurry after stirring 15min.
The sodium metaaluminate of 320.8kg is prepared by mixing into 1.9m with sodium hydroxide and water3Sodium aluminate solution, its In：Al2O3Mass concentration for 105g/L, NaOH mass concentration be 235g/L, by sodium aluminate solution according to 55L/min speed Degree is at the uniform velocity added in the second slurry and stirs 45min and obtains the 3rd slurry, and now slurry pH value is 9.2.
0.15m is prepared by mixing into the second aluminum sulfate of 52.8kg and sulphuric acid and water3The second aluminum sulfate solution, wherein： Al2O3Mass concentration be 105g/L, H2SO4Mass concentration be 190g/L, the second aluminum sulfate solution is added to the 3rd slurry In and stir 30min and obtain the 4th slurry, the pH of the 4th slurry is 7.6.
4th slurry is continued stirring 150min, inorganic coating terminates to obtain the 5th slurry.5th slurry is used resistance Rate carries out washing for the desalted water of 210K Ω and obtains filter cake.Filter cake drying is obtained middle by product.Using pressure it is 21MPa, temperature is that 300 DEG C of steam is crushed to intermediate product, adds the octyltri-ethoxysilane of 0.18t while crushing Obtain titanium dioxide.
Embodiment 3
At a temperature of 55 DEG C, 27t titanium dioxide base material is mixed with water, be dispersed through, wet grinding, classification are prepared into mass concentration The ammonium dihydrogen phosphate of 0.033t is added for Titanium dioxide slurry that 300g/l, pH value are 8.3 and in Titanium dioxide slurry, is kept stirring for Titanium dioxide slurry 25min.
The Disulfatozirconic acid. of 301.98kg is prepared into 1.25m with sulphuric acid and water reaction3Sulphuric acid zirconium solution, wherein：ZrO2's Mass concentration is 105g/L, H2SO4Mass concentration is 270g/L, and sulphuric acid zirconium solution is at the uniform velocity added titanium white according to 26L/min speed In slurry material and stir 45min and obtain the first slurry.
First aluminum sulfate of 362.6kg is prepared into 1.03m with sulphuric acid and water reaction3The first aluminum sulfate solution, its In：Al2O3Mass concentration be 105g/L, H2SO4Mass concentration be 200g/L, by the first aluminum sulfate solution according to 100L/ Min speed is at the uniform velocity added in the first slurry and obtains the second slurry after stirring 15min.
The sodium metaaluminate of 287kg is prepared into 1.7m with sodium hydroxide and water reaction3Sodium aluminate solution, wherein： Al2O3Mass concentration for 105g/L, NaOH mass concentration be 240g/L, sodium aluminate solution is even according to 60L/min speed Speed adds in the second slurry and stirs 45min and obtain the 3rd slurry, and now slurry pH value is 9.5.
0.14m is prepared by mixing into the second aluminum sulfate of 49.3kg and sulphuric acid and water3The second aluminum sulfate solution, wherein： Al2O3Mass concentration be 105g/L, H2SO4Mass concentration be 210g/L, the second aluminum sulfate solution is added to the 3rd slurry In and stir 30min and obtain the 4th slurry, the pH of the 4th slurry is 7.7.
4th slurry is continued stirring 100min, inorganic coating terminates to obtain the 5th slurry.5th slurry is used resistance Rate carries out washing for the desalted water of 203K Ω and obtains filter cake.Filter cake drying is obtained middle by product.Using pressure it is 18MPa, temperature is that 300 DEG C of steam is crushed to intermediate product, adds the octyltri-ethoxysilane of 0.22t while crushing Obtain titanium dioxide.
Embodiment 4
At a temperature of 57 DEG C, 24t titanium dioxide base material is mixed with water, be dispersed through, wet grinding, classification are prepared into mass concentration The ammonium dihydrogen phosphate of 0.03t is added for Titanium dioxide slurry that 290g/l, pH value are 8.2 and in Titanium dioxide slurry, is kept stirring for Titanium dioxide slurry 25min.
The Disulfatozirconic acid. of 273.3kg is prepared into 1.08m with sulphuric acid and water reaction3Sulphuric acid zirconium solution, wherein：ZrO2's Mass concentration is 110g/L, H2SO4Mass concentration is 285g/L, and sulphuric acid zirconium solution is at the uniform velocity added titanium white according to 28L/min speed In slurry material and stir 45min and obtain the first slurry.
First aluminum sulfate of 336.4kg is prepared into 0.912m with sulphuric acid and water reaction3The first aluminum sulfate solution, its In：Al2O3Mass concentration be 110g/L, H2SO4Mass concentration be 195g/L, by the first aluminum sulfate solution according to 110L/ Min speed is at the uniform velocity added in the first slurry and obtains the second slurry after stirring 15min.
The sodium metaaluminate of 267kg is prepared into 1.51m with sodium hydroxide and water reaction3Sodium aluminate solution, wherein： Al2O3Mass concentration for 110g/L, NaOH mass concentration be 230g/L, sodium aluminate solution is even according to 50L/min speed Speed adds in the second slurry and stirs 45min and obtain the 3rd slurry, and now slurry pH value is 9.1.
0.12m is prepared by mixing into the second aluminum sulfate of 44.3kg and sulphuric acid and water3The second aluminum sulfate solution, wherein： Al2O3Mass concentration be 110g/L, H2SO4Mass concentration be 210g/L, the second aluminum sulfate solution is added to the 3rd slurry In and stir 30min and obtain the 4th slurry, the pH of the 4th slurry is 7.4.
4th slurry is continued stirring 110min, inorganic coating terminates to obtain the 5th slurry.5th slurry is used resistance Rate carries out washing for the desalted water of 205K Ω and obtains filter cake.Filter cake drying is obtained middle by product.Using pressure it is 20MPa, temperature is that 290 DEG C of steam is crushed to intermediate product, adds the octyltri-ethoxysilane of 0.24t while crushing Obtain titanium dioxide.
Embodiment 5
At a temperature of 58 DEG C, 28t titanium dioxide base material is mixed with water, be dispersed through, wet grinding, classification are prepared into mass concentration The ammonium dihydrogen phosphate of 0.034t is added for Titanium dioxide slurry that 305g/l, pH value are 8.6 and in Titanium dioxide slurry, is kept stirring for Titanium dioxide slurry 25min.
The Disulfatozirconic acid. of 289.9kg is prepared into 1.26m with sulphuric acid and water reaction3Sulphuric acid zirconium solution, wherein：ZrO2's Mass concentration is 100g/L, H2SO4Mass concentration is 295g/L, and sulphuric acid zirconium solution is at the uniform velocity added titanium white according to 30L/min speed In slurry material and stir 45min and obtain the first slurry.
First aluminum sulfate of 358.8kg is prepared into 1.07m with sulphuric acid and water reaction3The first aluminum sulfate solution, its In：Al2O3Mass concentration be 100g/L, H2SO4Mass concentration be 205g/L, by the first aluminum sulfate solution according to 80L/min Speed is at the uniform velocity added in the first slurry and obtains the second slurry after stirring 15min.
The sodium metaaluminate of 283kg is prepared into 1.76m with sodium hydroxide and water reaction3Sodium aluminate solution, wherein： Al2O3Mass concentration for 100g/L, NaOH mass concentration be 245g/L, sodium aluminate solution is even according to 55L/min speed Speed adds in the second slurry and stirs 45min and obtain the 3rd slurry, and now slurry pH value is 9.
0.14m is prepared by mixing into the second aluminum sulfate of 46.9kg and sulphuric acid and water3The second aluminum sulfate solution, wherein： Al2O3Mass concentration be 100g/L, H2SO4Mass concentration be 205g/L, the second aluminum sulfate solution is added to the 3rd slurry In and stir 30min and obtain the 4th slurry, the pH of the 4th slurry is 7.2.
4th slurry is continued stirring 130min, inorganic coating terminates to obtain the 5th slurry.5th slurry is used resistance Rate carries out washing for the desalted water of 200K Ω and obtains filter cake.Filter cake drying is obtained middle by product.Using pressure it is 19MPa, temperature is that 305 DEG C of steam is crushed to intermediate product, adds the octyltri-ethoxysilane of 0.21t while crushing Obtain titanium dioxide.
According to《GB T 1706-2006 TiO 2 pigment》Standard, enters to the performance of titanium dioxide prepared by embodiment 1～5 Row detection.Measurement result is shown in Table 1.
The performance detection index and result of 1. titanium dioxide of table
As it can be seen from table 1 this titanium dioxide has, glossiness height, good dispersion, oil absorption be low, hydrophobicity is good and blue The features such as bottom phase, especially in plastics, color masterbatch system, the compatibility is splendid, and mobility is preferable, and processing characteristics is superior, is a kind of excellent Plastics titanium dioxide.
Embodiments described above is a part of embodiment of the present invention, rather than whole embodiments.The reality of the present invention The detailed description for applying example is not intended to limit the scope of claimed invention, but is merely representative of the selected enforcement of the present invention Example.Based on the embodiment in the present invention, those of ordinary skill in the art are obtained under the premise of creative work is not made Every other embodiment, belongs to the scope of protection of the invention.

Claims (10)

1. a kind of preparation method of titanium dioxide, it is characterised in which includes：
According to the mass fraction, by 88～111 parts of titanium dioxide base material be prepared into Titanium dioxide slurry and successively with 0.45～0.55 part Sulphuric acid zirconium solution, 0.35～0.45 part of the first aluminum sulfate solution, 0.6～0.7 part of sodium aluminate solution and 0.04～ 0.06 part of the second aluminum sulfate solution mixing, wash and be dried to obtain intermediate product, by the intermediate product and 0.06～ 0.08 part of silane coupler is mixed to get the titanium dioxide.
2. the preparation method of titanium dioxide according to claim 1, it is characterised in that the Titanium dioxide slurry is by following methods It is obtained：The titanium dioxide base material is dispersed through, wet grinding, classification obtain the Titanium dioxide slurry, in the Titanium dioxide slurry, TiO2 Mass concentration be 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l, pH value be 9～10.5 280～320g/l,.
3. the preparation method of titanium dioxide according to claim 2, it is characterised in that also include to the titanium during dispersion The step of dispersant being added in white lead dispersion liquid, the dispersant is selected from monoisopropanolamine, sodium silicate and Polymeric sodium metaphosphate. extremely Few one kind, in the divided titanium dioxide dispersion liquid, TiO2Mass concentration >=600g/L, pH value be 9～11.
4. the preparation method of titanium dioxide according to claim 2, it is characterised in that after the classification, the titanium dioxide slurry In material, TiO2Granularity be 0.2～0.3 μm.
5. the preparation method of titanium dioxide according to claim 1, it is characterised in that the matter of sulphuric acid in the sulphuric acid zirconium solution Amount concentration is 190～210g/L, total iron content≤30ppm.
6. the preparation method of titanium dioxide according to claim 1, it is characterised in that sulphuric acid in first aluminum sulfate solution Mass concentration be 270～300g/L, total iron content≤30ppm.
7. the preparation method of titanium dioxide according to claim 1, it is characterised in that sulphuric acid in second aluminum sulfate solution Mass concentration be 270～300g/L, total iron content≤30ppm.
8. the preparation method of titanium dioxide according to claim 1, it is characterised in that the hydrogen in the sodium aluminate solution Sodium oxide mass concentration is 230～245g/L, total iron content≤30ppm.
9. the preparation method of titanium dioxide according to claim 1, it is characterised in that in also including to institute's Titanium dioxide slurry plus Enter 0.03～0.036 mass parts ammonium dihydrogen phosphate the step of.
10. a kind of titanium dioxide, it is characterised in that the preparation method system of the titanium dioxide according to any one of claim 1～9 ?.
CN201610796961.7A 2016-08-31 2016-08-31 Titanium dioxide and preparing method thereof Pending CN106433226A (en)

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CN106947296A (en) * 2017-04-26 2017-07-14 攀钢集团研究院有限公司 High-weatherability titanium dioxide and preparation method thereof
CN107063947A (en) * 2017-04-28 2017-08-18 攀钢集团研究院有限公司 The method that particle size analyzer tests plastics special titanium pigment granularity
CN108003662A (en) * 2017-11-30 2018-05-08 广西雅照钛白有限公司 A kind of titanium dioxide and its manufacture method
CN108948799A (en) * 2018-07-10 2018-12-07 四川龙蟒钛业股份有限公司 A kind of production method of top grade color masterbatch grade titanium dioxide
CN108997789A (en) * 2018-09-05 2018-12-14 攀枝花大互通钛业有限公司 A kind of compound modified titanium and preparation method thereof
CN112885180A (en) * 2021-02-02 2021-06-01 内蒙古国城资源综合利用有限公司 Titanium white device typical control loop simulation training system and method
CN116023806A (en) * 2022-09-22 2023-04-28 攀枝花东方钛业有限公司 Titanium dioxide for environment-friendly paint and preparation method thereof

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CN102070921A (en) * 2010-12-25 2011-05-25 锦州钛业有限公司 Method for preparing special titanium dioxide pigment for plastic sectional materials by chlorination method
CN103112891A (en) * 2013-02-25 2013-05-22 南京钛白化工有限责任公司 Preparation method of high-performance rutile titanium white

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CN101463195A (en) * 2007-12-21 2009-06-24 衡阳天友化工有限公司 Rutile type titanium dioxide coating method and preparation method of used reagent
CN102070921A (en) * 2010-12-25 2011-05-25 锦州钛业有限公司 Method for preparing special titanium dioxide pigment for plastic sectional materials by chlorination method
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106947296A (en) * 2017-04-26 2017-07-14 攀钢集团研究院有限公司 High-weatherability titanium dioxide and preparation method thereof
CN107063947A (en) * 2017-04-28 2017-08-18 攀钢集团研究院有限公司 The method that particle size analyzer tests plastics special titanium pigment granularity
CN108003662A (en) * 2017-11-30 2018-05-08 广西雅照钛白有限公司 A kind of titanium dioxide and its manufacture method
CN108948799A (en) * 2018-07-10 2018-12-07 四川龙蟒钛业股份有限公司 A kind of production method of top grade color masterbatch grade titanium dioxide
CN108997789A (en) * 2018-09-05 2018-12-14 攀枝花大互通钛业有限公司 A kind of compound modified titanium and preparation method thereof
CN112885180A (en) * 2021-02-02 2021-06-01 内蒙古国城资源综合利用有限公司 Titanium white device typical control loop simulation training system and method
CN116023806A (en) * 2022-09-22 2023-04-28 攀枝花东方钛业有限公司 Titanium dioxide for environment-friendly paint and preparation method thereof

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