CN106833028A - A kind of production method of high coloring power pigment-level titanium brown - Google Patents

A kind of production method of high coloring power pigment-level titanium brown Download PDF

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CN106833028A
CN106833028A CN201611150594.XA CN201611150594A CN106833028A CN 106833028 A CN106833028 A CN 106833028A CN 201611150594 A CN201611150594 A CN 201611150594A CN 106833028 A CN106833028 A CN 106833028A
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titanium dioxide
slurry
meter
brown
production method
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CN106833028B (en
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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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    • 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
    • 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
    • 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
    • C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • 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
    • C09C3/06—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
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/08—Treatment with low-molecular-weight non-polymer organic 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
    • C09C3/12—Treatment with organosilicon compounds

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  • Organic Chemistry (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention discloses a kind of production method of high coloring power pigment-level titanium brown.The present invention utilizes the high reaction activity of nanoscale hydrated titanium dioxide, from suitable nanoscale hydrated titanium dioxide, based on this hydrated titanium dioxide, addition titanic acid-sol, Zn-ef ficiency, antimony oxide, aluminium salt, phosphoric acid, the additive treatings such as chromium oxide, by high-temperature calcination, crush, desalination is obtained product pigment-level titanium brown.The pigment has particle diameter small and is distributed the strong notable feature of concentrations, bright-colored, easy dispersion, colorability, is the outstanding upgrading substitute of commercial brown color pigment at present.

Description

A kind of production method of high coloring power pigment-level titanium brown
Technical field
The present invention relates to the preparation method of titanium brown, high coloring is prepared more particularly, to using suitable nanoscale hydrated titanium dioxide The production method of power pigment-level titanium brown.
Background technology
Environmental protection is paid attention to increasingly both at home and abroad at present, containing heavy metal and poisonous carcinogenic pigment, in the whole world, limitation makes With.Although expensive and organic pigment is free of extremely toxic substance.Traditional pigment, whether organic pigment or inorganic face Material, does not have the performances such as heat-resisting, fast light, weather-proof, acid and alkali-resistance and solvent resistant concurrently, it is impossible to complete adaptive functions coating and plastics should With requiring.It is the current preferable upgrading substitute with brown color pigment and titanium brown pigment then has more comprehensive application performance.
The excellent properties that titanium brown pigment has：1. due to being got by pyroreaction and calcining, crystal formation and lattice structure phase When stabilization, heat-resisting, fast light, weather-proof and resistance to various chemical mediator performances are very excellent, and resistance to chalking can exceed that any pale brown Color pigment.2. because with hardness and proportion higher very high, titanium brown pigment is in the case of it can provide high covering power and can be in Existing wearability very high.3. titanium brown pigment has neutral pH value, it is adaptable to various medium systems, will not be risen with medium system anti- Should.4. titanium brown pigment easily disperses, and with anti-migrating property, bleeding phenomenon does not occur.Although 5. titanium brown pigment contains color development element, These elements enter TiO2Lattice, the safety body of innoxious requirement is not completely suitable under general condition by any medium etch System, such as child plastic toy and all coating, packaging material for food, medical supplies, cosmetics, sanitary ware.
Solid phase method technique being used the more ripe titanium brown product of in the market, with titanium dioxide as primary raw material, although technique more Relatively simple, cost is relatively low, but due to titanium dioxide be stabilization crystal structure, it is necessary to temperature higher carries out solid oxidation Thing mixed calcining, causes product cut size to be difficult to control, and disperses uneven, and tinting strength, tinting power is poor, and color and luster is not vivid enough, therefore titanium brown Range of application is subject to a definite limitation.The production of titanium brown, thing are carried out for primary raw material using nanoscale high activity hydrated titanium dioxide The other mixing of molecular level is realized between material, is that a kind of simple and easy to do and product quality stablizes controllable production method.
The content of the invention
The purpose of the present invention, is to provide for a kind of production method of titanium brown pigment, and the technical problem that the method is solved is Using nanoscale hydrated titanium dioxide high reaction activity the characteristics of, by preferred nanoscale high activity hydrated titanium dioxide, right Hydrated titanium dioxide is once washed, acid treatment, secondary washing, plus inorganic agent mixing, calcining, once crush, grinding desalination, The key steps such as dry, steam flow crushing, to reach the purpose of output high-quality titanium brown.
The production method that the present invention is provided comprises the steps：
A, hydrated titanium dioxide are once washed：Choose hydrolysate hydration titanium dioxide prepared by sulfate process titanium dioxide production technology Titanium, sedimentation rate index meets 90~130mm/30min, and hydrated titanium dioxide is washed with 55~70 DEG C of running water, washing Qualified Judging index is that the iron content (in terms of Fe) in a washing waste water is less than 100mg/L；
B, acid treatment：Gained hydrated titanium dioxide will once be washed plus running water will be made slurry, titanium dioxide concentration control Be 260~340g/L, temperature at 55~70 DEG C, with H2SO4Meter, addition sulfuric acid is 25~50g/L, with Ti2O3Count, titanous is 0.5~1.5g/L, processes slurry 1~2 hour with this understanding；After treatment terminates, calcining seeds, TiO in calcining seeds are added2 Quality account for contained TiO in pending slurry2The 0.0~5.0% of quality, stirs 30 minutes；
The calcining seeds are titanic acid-sol calcining seeds, and the titanic acid-sol calcining seeds are given birth to for sulfate process titanium dioxide Rutile type calcining seeds prepared by production. art；
The secondary washing of c, hydrated titanium dioxide：With 55~70 DEG C of desalted waters hydrated titanium dioxide good to step b acid treatments Slurry is washed, and it is iron content in secondary washing waste water (with Fe to wash qualified Judging index2O3Meter) control be less than 10mg/L；
D, plus inorganic agent：Add desalted water to adjust titanium dioxide concentration in secondary washing gained hydrated titanium dioxide slurry to control It is 260~340g/L；Slurry pH value to 2.5~4.0 is adjusted with alkali；To account for contained TiO in pending slurry2The mass fraction of amount Meter, with Sb2O3Meter, the adding proportion of the antimony oxide of addition is 10~15%；With Cr2O3Meter, the adding proportion of chromium oxide for 8~ 15%；With H3PO4Meter, the adding proportion of phosphoric acid is 0.00~0.25%；With Al2O3The adding proportion of meter, aluminum sulfate or aluminium chloride It is 0.00~0.3%；In terms of ZnO, the adding proportion of zinc oxide or zinc sulfate or zinc chloride is 0.0~0.5%；In terms of MgO, oxygen The adding proportion for changing magnesium or magnesium sulfate or magnesium chloride is 0.0~0.5%；Slurry is stirred after adding mentioned reagent 0.5~1 hour, Slurry is pressed dry into moisture standby；
E, calcining：The material that moisture will be pressed dry is calcined, and highest calcining heat is controlled between 900~1200 DEG C, is forged Rutile-type crystal formation content >=98.5% in burning product；
F, crushing：Calcining product are crushed with pulverizer, 45 μm of residue on sieves of control smashing fineness are less than 0.05%, obtain final product Titanium brown primary product；
G, desalination, sand milling：Titanium brown primary product are made slurry with desalted water, slurry is ground with sand mill, selected With 0.6~0.8 μm of zirconium silicate pearl or yttrium stabilised zirconia pearl, the slurry after grinding is washed with desalted water, control washing is useless Water conductivity is less than 80 μm/cm, slurry is pressed dry into moisture standby；
H, drying, steam flow are crushed：The drying materials that moisture will be pressed dry remove moisture removal, add trimethylolethane, three hydroxyl first Base propane, polydimethylsiloxanepolymer polymer one kind therein, addition is account for comminuting matter quality 0.1~0.8%, through vapour Stream crushes to obtain titanium brown product.
Beneficial effects of the present invention：
(1) products obtained therefrom of the present invention is rutile-type crystal structure, and with preferable particle diameter distribution, particle diameter D50 is between 250 Between~400nm, product has excellent dispersiveness, tinting strength, tinting power higher.The method is hydrated by preferred nanoscale high activity Titanium dioxide simultaneously adds color development element, auxiliary agent after carrying out removal of impurities to it so that the size tunable of titanium brown product is grown up；It is logical Crossing carries out desalination, grinding to titanium brown primary product and adds different surfactants, may be such that product has widely suitable The property used.
(2) present invention process is simple, easy to operate, with low cost.
Specific embodiment
With reference to specific embodiment, the present invention is further illustrated, but protection scope of the present invention is not limited to This.
Embodiment 1
The hydrolysate hydrated titanium dioxide of sulfate process titanium dioxide production technology preparation is taken, sedimentation rate is 130mm/30min, with 60~65 DEG C of running water are washed to hydrated titanium dioxide, iron content (in terms of the Fe) 95mg/L in a washing waste water；Will Once washing gained hydrated titanium dioxide adds running water to be made slurry, and concentration is 338g/L, and temperature adds sulfuric acid at 60~65 DEG C (with H2SO4Meter) it is 45g/L, titanous is (with Ti2O3Meter) it is 0.8g/L, it is contained in pending slurry to account for after processing 1 hour The mass fraction meter of TiO2 amounts, adds titanic acid-sol calcining seeds (with TiO2Meter), adding proportion is 5.0%；With 55~60 DEG C desalted water hydrated titanium dioxide good to acid treatment is washed, and the iron content in secondary washing waste water is (with Fe2O3Meter) be 8mg/L；Desalted water is added to be made slurry secondary washing gained hydrated titanium dioxide, concentration is 335g/L；Adjusted with potassium hydroxide Slurry pH value is to 2.5~4.0；To account for contained TiO in pending slurry2The mass fraction meter of amount, the antimony oxide of addition is (with Sb2O3 Meter) adding proportion be 10%；Chromium oxide is (with Cr2O3Meter) adding proportion be 8%；Phosphoric acid (in terms of H3PO4) adding proportion is 0.00%；Aluminum sulfate or aluminium chloride are (with Al2O3Meter) adding proportion be 0.1%；Stirred 0.5~1 hour after adding mentioned reagent, Slurry is pressed dry into moisture content to be calcined, highest calcining heat is controlled at 1200 DEG C, and rutile-type crystal formation content is in calcining product 99.5%；Calcining product are crushed with mechanical crusher, smashing fineness 0.02% obtains final product titanium brown primary product；By at the beginning of titanium brown Level product is made slurry with desalted water, and slurry is ground with sand mill, from 0.6~0.8 μm of zirconium silicate pearl, uses desalination Water is washed to the slurry after grinding, 80 μm/cm of washing waste water electrical conductivity, and slurry is pressed dry into moisture；The thing of moisture will be pressed dry Moisture removal is removed in material drying, adds trimethylolethane, and addition is account for comminuting matter quality 0.1%, and titanium is crushed to obtain through steam flow Brown product.
Embodiment 2
The hydrolysate hydrated titanium dioxide of sulfate process titanium dioxide production technology preparation is taken, sedimentation rate is 92mm/30min, with 55~60 DEG C of running water are washed to hydrated titanium dioxide, iron content (in terms of the Fe) 85mg/L in a washing waste water；Will Once washing gained hydrated titanium dioxide adds running water to be made slurry, and concentration is 260g/L, and temperature adds sulfuric acid at 55~60 DEG C (with H2SO4Meter) it is 27g/L, titanous is (with Ti2O3Meter) it is 1.5g/L, it is contained in pending slurry to account for after processing 2 hours TiO2The mass fraction meter of amount, adds titanic acid-sol calcining seeds (with TiO2Meter), adding proportion is 0.0%；With 60~65 DEG C The desalted water hydrated titanium dioxide good to acid treatment is washed, and the iron content in secondary washing waste water is (with Fe2O3Meter) be 10mg/L；Desalted water is added to be made slurry secondary washing gained hydrated titanium dioxide, concentration is 265g/L；Adjusted with potassium carbonate and starched Expect pH value to 2.5~4.0；To account for contained TiO in pending slurry2The mass fraction meter of amount, the antimony oxide of addition is (with Sb2O3 Meter) adding proportion be 15%；Chromium oxide is (with Cr2O3Meter) adding proportion be 15%；Phosphoric acid is (with H3PO4Meter) adding proportion is 0.25%；Zinc oxide or zinc sulfate or zinc chloride (being counted with ZnO) adding proportion are 0.5%；Add stirring 0.5 after mentioned reagent~ 1 hour, slurry is pressed dry into moisture content and is calcined, highest calcining heat is controlled at 900 DEG C, rutile-type crystal formation content in calcining product It is 98.5%；Calcining product are crushed with mechanical crusher, smashing fineness 0.01% obtains final product titanium brown primary product；By titanium brown Primary product are made slurry with desalted water, and slurry is ground with sand mill, from 0.6~0.8 μm of yttrium stabilised zirconia pearl, use Desalted water is washed to the slurry after grinding, 75 μm/cm of washing waste water electrical conductivity, and slurry is pressed dry into moisture；Moisture will be pressed dry Drying materials remove moisture removal, add trimethylolpropane, addition is account for comminuting matter quality 0.3%, is crushed through steam flow Obtain titanium brown product.
Embodiment 3
The hydrolysate hydrated titanium dioxide of sulfate process titanium dioxide production technology preparation is taken, sedimentation rate is 115mm/30min, with 60~65 DEG C of running water are washed to hydrated titanium dioxide, iron content (in terms of the Fe) 85mg/L in a washing waste water；Will Once washing gained hydrated titanium dioxide adds running water to be made slurry, and concentration is 300g/L, and temperature adds sulfuric acid at 65~70 DEG C (with H2SO4Meter) it is 36g/L, titanous is (with Ti2O3Meter) it is 1.1g/L, it is contained in pending slurry to account for after processing 1.5 hours TiO2The mass fraction meter of amount, adds titanic acid-sol calcining seeds (with TiO2Meter), adding proportion is 1.0%；With 65~70 DEG C The desalted water hydrated titanium dioxide good to acid treatment is washed, and the iron content in secondary washing waste water is (with Fe2O3Meter) it is 9mg/ L；Desalted water is added to be made slurry secondary washing gained hydrated titanium dioxide, concentration is controlled to 285g/L；Adjusted with NaOH Slurry pH value is to 2.5~4.0；To account for contained TiO in pending slurry2The mass fraction meter of amount, the antimony oxide of addition is (with Sb2O3 Meter) adding proportion be 12%；Chromium oxide is (with Cr2O3Meter) adding proportion be 12%；Phosphoric acid is (with H3PO4Meter) adding proportion is 0.05%；Aluminum sulfate or aluminium chloride are (with Al2O3Meter) adding proportion be 0.2%；Zinc oxide or zinc sulfate or zinc chloride are (with ZnO Meter) adding proportion be 0.2%；Magnesia or magnesium sulfate or magnesium chloride adding proportion are 0.5%；Stirred after adding mentioned reagent 0.5~1 hour, slurry is pressed dry into moisture content and is calcined, highest calcining heat is controlled at 1000 DEG C, rutile-type is brilliant in calcining product Type content >=99.0%；Calcining product are crushed with mechanical crusher, smashing fineness 0.03% obtains final product titanium brown primary product； Titanium brown primary product are made slurry with desalted water, slurry is ground with sand mill, from 0.6~0.8 μm of zirconium silicate Pearl, is washed with desalted water to the slurry after grinding, 80 μm/cm of washing waste water electrical conductivity, and slurry is pressed dry into moisture；To press dry The drying materials of moisture content remove moisture removal, add polydimethylsiloxanepolymer polymer, and addition is to account for comminuting matter quality 0.8%, crush to obtain titanium brown product through steam flow.
Titanium brown product to embodiment detects that R% therein is XRD testing results, and particle diameter is examined for laser particle analyzer Result is surveyed, the examination criteria of tinting strength, tinting power is GB/T13451.2-92《Coloring pigment relative color strength and the relative scattering of Chinese white The measure photometer measuring method of power》, gained detection data listed in table 1 later：
Table 1：Embodiment Product checking data

Claims (9)

1. a kind of production method of high coloring power pigment-level titanium brown, it is characterised in that comprise the following steps：
A, hydrated titanium dioxide are once washed：Take the qualified hydrolysate hydration titanium dioxide of sulfate process titanium dioxide production technology preparation Titanium, is washed with 50~60 DEG C of running water to hydrated titanium dioxide, washes qualified Judging index in a washing waste water Iron content (in terms of Fe) be less than 100mg/L；
B, acid treatment：Gained hydrated titanium dioxide will once be washed plus running water will be made slurry, titanium dioxide concentration will be controlled to 260 ~340g/L, temperature at 55~70 DEG C, with H2SO4Meter, addition sulfuric acid is 25~50g/L, with Ti2O3Meter, titanous be 0.5~ 1.5g/L, processes slurry 1~2 hour with this understanding；After treatment terminates, calcining seeds, TiO in calcining seeds are added2Matter Measure to account for contained TiO in pending slurry2The 0.0~5.0% of quality, stirs 30 minutes after adding；
The secondary washing of c, hydrated titanium dioxide：With 55~70 DEG C of desalted waters hydrated titanium dioxide slurry good to step b acid treatments Washed, it is iron content in secondary washing waste water (with Fe to wash qualified Judging index2O3Meter) control less than 10mg/ L；
D, plus inorganic agent：Add desalted water to adjust titanium dioxide concentration in secondary washing gained hydrated titanium dioxide slurry to be controlled to 260~340g/L；Slurry pH value to 2.5~4.0 is adjusted with alkali；To account for contained TiO in pending slurry2The mass fraction of amount Meter, with Sb2O3Meter, antimony oxide adding proportion is 10~15%；With Cr2O3Meter, the adding proportion of chromium oxide is 8~15%；With H3PO4Meter, the adding proportion of phosphoric acid is 0.00~0.25%；With Al2O3Meter, the adding proportion of silicon source is 0.00~0.3%, with ZnO is counted, and the adding proportion in zinc source is 0.0~0.5%；In terms of MgO, magnesium source adding proportion is 0.0~0.5%；Add above-mentioned examination Stirred 0.5~1 hour after agent, slurry is pressed dry into moisture standby；
E, calcining：The material that moisture will be pressed dry is calcined, and highest calcining heat is controlled between 900~1200 DEG C, calcines product Middle rutile-type crystal formation content >=98.5%；
F, crushing：Calcining product are crushed with pulverizer, control smashing fineness is qualified, obtains final product titanium brown primary product；
G, desalination, sand milling：Titanium brown primary product are made slurry with desalted water, slurry is ground with sand mill, from 0.6 ~0.8 μm of zirconium silicate pearl or yttrium stabilised zirconia pearl, is washed with desalted water to the slurry after grinding, controls washing waste water conductance Rate is less than 80 μm/cm, slurry is pressed dry into moisture standby；
H, drying, steam flow are crushed：The drying materials that moisture will be pressed dry remove moisture removal, add surface conditioning agent, are crushed through steam flow Titanium brown product.
2. a kind of production method of the high coloring power pigment-level titanium brown according to claims 1, it is characterised in that step a In, qualified hydrolysate hydrated titanium dioxide prepared by the sulfate process titanium dioxide production technology refers to hydrolysate sedimentation rate index Meet the hydrolysis material of 90~130mm/30min；The measuring method of hydrolysate sedimentation rate index is：100ml is taken more than 90 DEG C Hydrolysate and 900ml temperature be sufficiently mixed for 20 ± 2 DEG C of desalted water after, be placed in 1000ml graduated cylinders, in 22 ± 2 DEG C Standing sedimentation 30min under environment, the supernatant liquor measured highly is the hydrolysate sedimentation rate.
3. a kind of production method of the high coloring power pigment-level titanium brown according to claims 1, it is characterised in that step b In, the titanic acid-sol calcining seeds are rutile type calcining seeds prepared by sulfate process titanium dioxide production technology.
4. a kind of production method of the high coloring power pigment-level titanium brown according to claims 1 or 2, it is characterised in that institute State desalted water and meet electrical conductivity less than 10 μ s/cm, clear appearance is transparent.
5. the production method of a kind of high coloring power pigment-level titanium brown according to claim 1, it is characterised in that in step d, The alkali be potassium hydroxide, potassium carbonate, NaOH, sodium carbonate, ammoniacal liquor it is therein one or more；The antimony oxide refers to content (with Sb2O3Meter) >=99.0%, the industrial goods antimony oxide of residue on sieve (mass fraction, 45 μm)≤0.05%；The chromium oxide refers to and contains Amount is (with Cr2O3Meter) >=99%, the industrial goods chromium oxide of residue on sieve (mass fraction, 45 μm)≤0.01%.
6. the production method of a kind of high coloring power pigment-level titanium brown according to claim 1, it is characterised in that in step d, Source of aluminium is aluminum sulfate or aluminium chloride；Zinc source is zinc oxide, zinc sulfate or zinc chloride；Magnesium source is magnesia, magnesium sulfate or chlorine Change magnesium.
7. the production method of a kind of high coloring power pigment-level titanium brown according to claim 1, it is characterised in that in step f, The smashing fineness is qualified, and it refers to that 45 μm of residue on sieves are less than 0.05% to obtain final product titanium brown primary product, and grain is detected through laser particle analyzer Footpath D50 between 250~400nm, rutile-type crystal formation content >=98.5%.
8. the production method of a kind of high coloring power pigment-level titanium brown according to claim 1, it is characterised in that in step h, The surface conditioning agent is trimethylolethane, trimethylolpropane, polydimethylsiloxanepolymer polymer one kind therein, addition Measure to account for the 0.1~0.8% of comminuting matter quality.
9. the production method of a kind of high coloring power pigment-level titanium brown according to claim 1, it is characterised in that in step h, The titanium brown product refers to 45 μm of residue on sieves less than 0.02%, through laser particle analyzer detection particle diameter D50 between 250~350nm it Between, water dissolvable salt content is less than 0.1%, rutile-type crystal formation content >=98.5%.
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Cited By (2)

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CN107652713A (en) * 2017-10-20 2018-02-02 攀钢集团攀枝花钢铁研究院有限公司 A kind of method for preparing titanium yellow pigment
CN107686346A (en) * 2017-09-11 2018-02-13 佛山市三水区百昕化工有限公司 The preparation method and ceramic pigment of a kind of ceramic pigment

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