CN106221297A - The method improving the surface organic process of titanium dioxide dispersibility - Google Patents

The method improving the surface organic process of titanium dioxide dispersibility Download PDF

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Publication number
CN106221297A
CN106221297A CN201610586610.3A CN201610586610A CN106221297A CN 106221297 A CN106221297 A CN 106221297A CN 201610586610 A CN201610586610 A CN 201610586610A CN 106221297 A CN106221297 A CN 106221297A
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titanium dioxide
organic process
surface organic
suspension
dispersibility
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CN106221297B (en
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刘婵
李礼
杜建桥
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Pangang Group Panzhihua Iron and Steel Research Institute Co Ltd
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Pangang Group Panzhihua Iron and Steel Research Institute Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36Compounds of titanium
    • C09C1/3607Titanium dioxide
    • C09C1/3669Treatment with low-molecular organic compounds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36Compounds of titanium
    • C09C1/3607Titanium dioxide
    • C09C1/3684Treatment with organo-silicon compounds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36Compounds of titanium
    • C09C1/3692Combinations of treatments provided for in groups C09C1/3615 - C09C1/3684
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006Combinations of treatments provided for in groups C09C3/04 - C09C3/12
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/08Treatment with low-molecular-weight non-polymer organic compounds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/12Treatment with organosilicon compounds

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The method that the present invention relates to a kind of surface organic process, more particularly to the method for the surface organic process of the performance improving Rutile type titanium dioxide, belongs to chemical field.For overcoming the defect of existing Rutile type titanium dioxide surface organic process method, preparing polymolecularity and the Rutile type titanium dioxide of high aqueous covering power, the method for the surface organic process that the present invention improves titanium dioxide dispersibility comprises the steps: a, the titanium dioxide after inorganic coating spends ionized water is prepared as titanium dioxide suspension;B, by suspension insulated and stirred;C, dropping aqueous citric acid solution, continue insulated and stirred;D, dropping organic agent, continue insulated and stirred;E, suspension is dried, and carries out comminution by gas stream.The rutile titanium white using this method to obtain has the inaccessiable good characteristic of other method, especially water dispersible and aqueous covering power, has good application and promotion prospect.

Description

The method improving the surface organic process of titanium dioxide dispersibility
Technical field
The method that the present invention relates to a kind of surface organic process, more particularly to the performance improving Rutile type titanium dioxide The method of surface organic process, belongs to chemical field.
Background technology
Titanium dioxide is important inorganic functional material, because of physics, the chemical property of its uniqueness, is widely used in painting The organic chemical industry fields such as material, plastics, papermaking, ink.Surface organic process can improve titanium dioxide and resin and organic solvent The compatibility, thus improve the application performance of titanium dioxide.
According to current pertinent literature report, in commercial production, organic agent adds in dry and comminution by gas stream two procedures Adding, adsorb on titanium dioxide surface in the way of physically or chemically, organic process effect is by the detection dispersibility of titanium dioxide, oil suction The pigment performance indexs such as amount, brightness and the application performance index such as covering power, glossiness characterize.Organic process influential effect is to titanium The indexs such as the dispersibility of white lead, the stability of oil absorption, and covering power.
In the Rutile type titanium dioxide surface organic process technology related to, not yet have and improve titanium white by pretreatment mode The organic process technology of powder surface organic process effect and method.
Summary of the invention
Present invention solves the technical problem that the defect being to overcome existing Rutile type titanium dioxide surface organic process method, Prepare polymolecularity and the Rutile type titanium dioxide of high aqueous covering power.
In order to solve above-mentioned technical problem, the method for the surface organic process that the present invention improves titanium dioxide dispersibility include as Lower step:
A, the titanium dioxide after inorganic coating is spent ionized water it is prepared as titanium dioxide suspension;
B, suspension is heated to 55~65 DEG C, insulated and stirred;
C, dropping aqueous citric acid solution, continue insulated and stirred, and wherein citric acid dosage is the 0.10% of titanium dioxide solid content ~0.20%;
D, dropping organic agent, continue insulated and stirred;
E, suspension is dried, and pulverizes.
Preferably, described in step b, c and d, the temperature of insulation is 60 DEG C.
Further, the suspension concentration of the titanium dioxide described in step a is 180~220g/L, preferably 200g/L.
Further, the time of the stirring described in step b is 20~40min, preferably 30min.
Further, the aqueous citric acid solution concentration described in step c is 40~60g/L.
Further, the mixing time 20~40min described in step c.
Further, the organic agent described in step d can be silicone oil emulsion, modified silicon oil emulsion, silane coupled At least one in agent and trimethylolpropane, wherein, organic agent dosage be titanium dioxide solids content 0.50%~ 1.00%.
Wherein, citric acid dosage: organic agent dosage=1: 5.
Further, the mixing time 20~40min described in step d.
Further, the suspension baking temperature described in step e is 105~120 DEG C, suspension be drying time 36~ 48h。
Compared with existing titanium dioxide organic process technology, the present invention uses citric acid that titanium dioxide is carried out pretreatment, passes through Chemical action, makes organic agent more stably overseas Chinese federation on titanium dioxide surface, is effectively increased organic agent at titanium dioxide table Face adsorption rate and absorption uniformity;On the premise of controlling citric acid dosage, the performance of product can be significantly improved, including dispersion Property, covering power and mobility etc..The rutile titanium white using this method to obtain has the inaccessiable good characteristic of other method, Especially water dispersible and aqueous covering power, have good application and promotion prospect.
Detailed description of the invention
The method of the surface organic process that the present invention improves titanium dioxide dispersibility comprises the steps:
A, the titanium dioxide after inorganic coating is spent ionized water it is prepared as titanium dioxide suspension;
B, suspension is heated to 55~65 DEG C, insulated and stirred;
C, dropping aqueous citric acid solution, continue insulated and stirred, and wherein citric acid dosage is the 0.10% of titanium dioxide solid content ~0.20%;
D, dropping organic agent, continue insulated and stirred;
E, suspension is dried, and pulverizes.
Wherein, when described in step b, c and d, the temperature of insulation is 60 DEG C, effect is best.
The suspension concentration of the titanium dioxide described in step a is unsuitable too high, also unsuitable on the low side, the suspension concentration of titanium dioxide Being advisable 180~220g/L, wherein the suspension concentration 200g/L effect of titanium dioxide is optimum.
The time of the stirring described in step b is that too short titanium dioxide granule is uneven, and the long production efficiency of mixing time is not Height, mixing time is advisable 20~40min, and mixing time 30min is optimal.
Further, the aqueous citric acid solution concentration described in step c is 40~60g/L.
Further, the mixing time 20~40min described in step c.
Further, the organic agent described in step d can be silicone oil emulsion, modified silicon oil emulsion, silane coupled At least one in agent and trimethylolpropane, the most preferably, organic agent dosage is titanium dioxide solids content 0.50%~1.00%.
Wherein, citric acid dosage: organic agent dosage=1: 5.
Further, the mixing time 20~40min described in step d.
Wherein, the suspension baking temperature described in step e is 105~120 DEG C, and suspension drying time is 36~48h, Wherein suspension baking temperature must not be higher than 120 DEG C;The drying time of suspension can be adjusted with baking temperature, temperature Gao Ze Drying time is few, and temperature is low, then drying time is long, and for example with the baking temperature of 105 DEG C, then drying time 48h, if used The drying temperature of 120 DEG C, then drying time 36h.
Below in conjunction with embodiment, the detailed description of the invention of the present invention is further described, the most therefore the present invention is limited System is among described scope of embodiments.
Embodiment 1
Taking the titanium dioxide after 200g inorganic coating, pull an oar with deionized water, the Titanium dioxide slurry concentration after making beating is 200g/ L, Titanium dioxide slurry heating in water bath to 60 DEG C, it is sufficiently stirred for 30min;
By the citric acid solution 4ml that above-mentioned slurry addition concentration is 50g/L, then it is sufficiently stirred for 30min, then presses titanium dioxide Solid content meter adds the silicone oil emulsion of 0.50%, is sufficiently stirred for 30min;
120 DEG C of slurry is dried 36h, carries out comminution by gas stream, obtain titanium dioxide product.
Detection obtains: the titanium dioxide oil-dispersing property of embodiment 1 is 6.50, water dispersible 44 μm, and aqueous covering power is 89.25%.
Embodiment 2
Taking the titanium dioxide after 200g inorganic coating, pull an oar with deionized water, the Titanium dioxide slurry concentration after making beating is 200g/ L, Titanium dioxide slurry heating in water bath to 60 DEG C, it is sufficiently stirred for 30min;
By the citric acid solution 8ml that above-mentioned slurry addition concentration is 50g/L, then it is sufficiently stirred for 30min, then presses titanium dioxide Solid content meter adds the hydroxyl modification organic silicon emulsion of 1.00%, is sufficiently stirred for 30min;
105 DEG C of slurry is dried 48h, carries out comminution by gas stream, obtain titanium dioxide product.
Detection obtains: titanium dioxide oil-dispersing property is 6.75, water dispersible 30 μm, and aqueous covering power is 92.88%.
Embodiment 3
Taking the titanium dioxide after 200g inorganic coating, pull an oar with deionized water, the Titanium dioxide slurry concentration after making beating is 220g/ L, Titanium dioxide slurry heating in water bath to 65 DEG C, it is sufficiently stirred for 20min;
Above-mentioned slurry will add the citric acid solution 4ml that concentration is 60g/L, then be sufficiently stirred for 20min, then press titanium white Powder solid content meter adds the organic silicon modified by polyether emulsion of 0.60%, is sufficiently stirred for 20min;
105 DEG C of slurry is dried 48h, carries out comminution by gas stream, obtain titanium dioxide product.
Detection obtains: titanium dioxide oil-dispersing property is 6.50, water dispersible 25 μm, and aqueous covering power is 91.55%.
Embodiment 4
Taking the titanium dioxide after 200g inorganic coating, pull an oar with deionized water, the Titanium dioxide slurry concentration after making beating is 180g/ L, Titanium dioxide slurry heating in water bath to 55 DEG C, it is sufficiently stirred for 40min;
Above-mentioned slurry will add the citric acid solution 7.5ml that concentration is 40g/L, then be sufficiently stirred for 40min, then press titanium White lead solid content meter adds the hydroxyl modification organic silicon emulsion of 0.75%, is sufficiently stirred for 40min;
105 DEG C of slurry is dried 48h, carries out comminution by gas stream, obtain titanium dioxide product.
Detection obtains: titanium dioxide oil-dispersing property is 6.50, water dispersible 35 μm, and aqueous covering power is 91.02%.
Comparative example 1
Comparative example 1 is the parallel test of embodiment 1, unique from embodiment 1 unlike comparative example 1 be added without concentration and be The citric acid solution 4ml of 50g/L, is sufficiently stirred for the step of 30min.
Detection obtains: the titanium dioxide oil-dispersing property 6.00 of comparative example 1, water dispersible 54 μm, and aqueous covering power is 85.05%.
Comparative example 2
Comparative example 2 is the parallel test of embodiment 2, unique from embodiment 2 unlike comparative example 2 be added without concentration and be The citric acid solution 8ml of 50g/L, then it is sufficiently stirred for the step of 30min.
Detection obtains: the titanium dioxide oil-dispersing property 6.25 of comparative example 2, water dispersible 44 μm, and aqueous covering power is 88.79%.
Visible, use the titanium dioxide moisture that the method for the surface organic process improving titanium dioxide dispersibility of the present invention prepares Dissipate property and aqueous covering power is the best, there is good application and promotion prospect.

Claims (10)

1. the method improving the surface organic process of titanium dioxide dispersibility, it is characterised in that comprise the steps:
A, the titanium dioxide after inorganic coating is spent ionized water it is prepared as titanium dioxide suspension;
B, suspension is heated to 55~65 DEG C, insulated and stirred;
C, dropping aqueous citric acid solution, continue insulated and stirred, wherein citric acid dosage be titanium dioxide solid content 0.10%~ 0.20%;
D, dropping organic agent, continue insulated and stirred;
E, suspension is dried, and pulverizes.
The method of the surface organic process of raising titanium dioxide dispersibility the most according to claim 1, it is characterised in that step The temperature 60 C of insulation described in b, c and d.
The method of the surface organic process of raising titanium dioxide dispersibility the most according to claim 1 and 2, it is characterised in that step The suspension concentration of the titanium dioxide described in rapid a is 180~220g/L, preferably 200g/L.
4. according to the method for the surface organic process improving titanium dioxide dispersibility described in any one of claim 13, its feature The time being the stirring described in step b is 20~40min, preferably 30min.
5. according to the method for the surface organic process improving titanium dioxide dispersibility described in any one of claim 14, its feature It is that the aqueous citric acid solution concentration described in step c is 40~60g/L.
6. according to the method for the surface organic process improving titanium dioxide dispersibility described in any one of claim 15, its feature It is citric acid dosage: organic agent dosage=1: 5.
7. according to the method for the surface organic process improving titanium dioxide dispersibility described in any one of claim 16, its feature It is the mixing time 20~40min described in step c.
8. according to the method for the surface organic process improving titanium dioxide dispersibility described in any one of claim 17, its feature It is that the organic agent described in step d is in silicone oil emulsion, modified silicon oil emulsion, silane coupler and trimethylolpropane At least one, wherein, organic agent dosage is the 0.50%~1.00% of titanium dioxide solid content.
9. according to the method for the surface organic process improving titanium dioxide dispersibility described in any one of claim 18, its feature It is the mixing time 20~40min described in step d.
10., according to the method for the surface organic process improving titanium dioxide dispersibility described in any one of claim 19, it is special Levying and be that the suspension baking temperature described in step e is 105~120 DEG C, suspension drying time is 36~48h.
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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107805410A (en) * 2017-11-24 2018-03-16 锦州钛业股份有限公司 A kind of titanium white production method improved in resin system dispersiveness
CN108384285A (en) * 2018-03-08 2018-08-10 四川龙蟒钛业股份有限公司 A kind of preparation method of high dispersive titanium dioxide
CN108587243A (en) * 2018-03-08 2018-09-28 四川龙蟒钛业股份有限公司 A kind of production method of high heap density color masterbatch grade titanium dioxide
CN108587247A (en) * 2018-07-10 2018-09-28 四川龙蟒钛业股份有限公司 A kind of production method of low VOC titanium dioxides
CN109438990A (en) * 2018-11-16 2019-03-08 山东道安新材料有限公司 A kind of compound silicone oil emulsion and preparation method thereof
CN110452560A (en) * 2019-08-28 2019-11-15 四川龙蟒钛业股份有限公司 A kind of production method of the high heap density color masterbatch grade titanium dioxide of high-temperature resistant
CN113387383A (en) * 2021-05-24 2021-09-14 龙佰四川钛业有限公司 Production method of high-fluidity titanium dioxide flash-dried material
CN113637354A (en) * 2021-07-30 2021-11-12 中建材(合肥)新能源有限公司 High-reflectivity water-based ink for photovoltaic module backboard glass
CN115124862A (en) * 2022-07-12 2022-09-30 攀钢集团重庆钒钛科技有限公司 Modified titanium dioxide and preparation method thereof
CN115746582A (en) * 2022-11-30 2023-03-07 攀钢集团研究院有限公司 Method for reducing oil absorption of titanium dioxide
CN115850998A (en) * 2022-11-30 2023-03-28 攀钢集团研究院有限公司 Method for improving brightness of titanium dioxide
CN115850999A (en) * 2022-11-30 2023-03-28 攀钢集团研究院有限公司 Preparation method of titanium dioxide for high-gloss high-dispersion ink

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CN1968894A (en) * 2004-02-26 2007-05-23 新型材料莱布尼兹研究所公益性有限责任公司 Amphiphilic nanoparticles
CN102993786A (en) * 2012-08-31 2013-03-27 道奇威(成都)科技有限公司 Organic surface modification method for improving water dispersion stability of rutile titanium dioxide

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CN1858309A (en) * 2006-01-10 2006-11-08 上海千泰高科技发展有限公司 Titanium white for dry acrylic spinning delustering its preparing method
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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107805410B (en) * 2017-11-24 2020-07-07 中信钛业股份有限公司 Titanium dioxide production method for improving dispersibility in resin system
CN107805410A (en) * 2017-11-24 2018-03-16 锦州钛业股份有限公司 A kind of titanium white production method improved in resin system dispersiveness
CN108384285A (en) * 2018-03-08 2018-08-10 四川龙蟒钛业股份有限公司 A kind of preparation method of high dispersive titanium dioxide
CN108587243A (en) * 2018-03-08 2018-09-28 四川龙蟒钛业股份有限公司 A kind of production method of high heap density color masterbatch grade titanium dioxide
CN108587247A (en) * 2018-07-10 2018-09-28 四川龙蟒钛业股份有限公司 A kind of production method of low VOC titanium dioxides
CN109438990A (en) * 2018-11-16 2019-03-08 山东道安新材料有限公司 A kind of compound silicone oil emulsion and preparation method thereof
CN110452560A (en) * 2019-08-28 2019-11-15 四川龙蟒钛业股份有限公司 A kind of production method of the high heap density color masterbatch grade titanium dioxide of high-temperature resistant
CN113387383A (en) * 2021-05-24 2021-09-14 龙佰四川钛业有限公司 Production method of high-fluidity titanium dioxide flash-dried material
CN113637354A (en) * 2021-07-30 2021-11-12 中建材(合肥)新能源有限公司 High-reflectivity water-based ink for photovoltaic module backboard glass
CN115124862A (en) * 2022-07-12 2022-09-30 攀钢集团重庆钒钛科技有限公司 Modified titanium dioxide and preparation method thereof
CN115124862B (en) * 2022-07-12 2023-11-10 攀钢集团重庆钒钛科技有限公司 Modified titanium dioxide and preparation method thereof
CN115746582A (en) * 2022-11-30 2023-03-07 攀钢集团研究院有限公司 Method for reducing oil absorption of titanium dioxide
CN115850998A (en) * 2022-11-30 2023-03-28 攀钢集团研究院有限公司 Method for improving brightness of titanium dioxide
CN115850999A (en) * 2022-11-30 2023-03-28 攀钢集团研究院有限公司 Preparation method of titanium dioxide for high-gloss high-dispersion ink

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