CN102515267A - Production method of high-resistivity titanium dioxide - Google Patents
Production method of high-resistivity titanium dioxide Download PDFInfo
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Abstract
The invention relates to a production method of high-resistivity titanium dioxide, which belongs to the field of titanium dioxide production. The invention provides the production method of the high-resistivity titanium dioxide, which adopts a sulfuric acid method titanium dioxide production process and comprises the following steps of hydrolyzation of titanium liquid, washing, salt treatment, and calcination plus milling, wherein a potassic substance is added in the salt treatment step; the addition quantity of the potassic substance occupies 0.39 to 0.47 wt% of the titanium dioxide content; and the potassic substance is potassic alkali or salt. The resistivity of the titanium dioxide produced by utilizing the method provided by the invention is higher than the resistivity of the titanium dioxide produced in the prior art by 900 Omega.cm, and meanwhile, the brightness, the whiteness, the pH (potential of hydrogen) of the titanium dioxide are guaranteed to satisfy the operation requirements.
Description
Technical field
The present invention relates to a kind of working method of high resistivity titanium white, belong to the titanium white production field.
Background technology
White titanium pigment (claiming titanium oxide again) has stable physics, chemical property and good optics, electrical properties and excellent pigment performance, therefore is widely used in industry such as coating, plastics, papermaking, printing-ink, chemical fibre, rubber, makeup.The working method of white titanium pigment mainly contains sulfuric acid process and chlorination.
Sulfuric acid process is to carry out acidolysis reaction with ilmenite concentrate or acid-dissolved titanium slag and sulfuric acid reaction, obtains titanyl sulfate solution, obtains the metatitanic acid deposition through hydrolysis, gets into rotary kiln calcining output TiO again
2Sulfuric acid process both can be produced the anatase titanium dioxide product, can produce the rutile-type product again.Titanium White Production By Sulfuric Acid Process comprises that mainly hydrolysis, washing, the salt of titanium liquid are handled, calcining powder process several steps, and the resistivity of the white titanium pigment that the existing sulfuric acid process of employing makes is 1600-2200 Ω cm, and indexs such as pH value, whiteness, brightness can reach application requiring basically.Because the white titanium pigment resistivity that existing method is produced is lower, can not be widely used in chemical fibre industry, contriver of the present invention is carrying out a large amount of research aspect the satisfactory high resistivity white titanium pigment of production over-all properties.
Summary of the invention
The technical problem that the present invention will solve provides a kind of method of producing the high resistivity white titanium pigment, and the gained white titanium pigment is high than the resistivity of the white titanium pigment that prior art is produced, and guarantees that simultaneously its brightness, form and aspect meet request for utilization.
Technical scheme of the present invention is:
The invention provides a kind of working method of high resistivity white titanium pigment, adopt the sulfuric acid method titanium pigment production technique, comprise the steps: that hydrolysis, washing, the salt of titanium liquid is handled, calcining powder process, wherein:
Add in the salt treatment step and contain the potassium material, the add-on that contains the potassium material accounts for the 0.39-0.47wt% of content of titanium dioxide, and wherein, containing the potassium material is potassic alkali or salt.
Preferably, the above-mentioned potassium material that contains is at least a in Pottasium Hydroxide, vitriolate of tartar, salt of wormwood, the potassiumphosphate.
Further, add phosphoric acid in the salt treatment step, the add-on of phosphoric acid accounts for the 0.28-0.3wt% of content of titanium dioxide.
Preferably, in the hydrolysing step of titanium liquid, get the metatitanic acid slurry after the hydrolysis, the median size of metatitanic acid is controlled at 1.5 μ m-1.7 μ m.
Preferably, in the salt treatment step, regulating the metatitanic acid slurry concentration is 300-340g/l.
Preferably, in the salt treatment step, add earlier and contain the potassium material, add phosphoric acid again.
Preferably, in the calcining powder process step, the metatitanic acid slurry after salt is handled carries out processed, makes its water cut be controlled to be 37-47wt%.
Beneficial effect of the present invention:
1, the white titanium pigment that utilizes the MV of the white titanium pigment resistivity that the inventive method produces to produce than prior art is up to 900 Ω cm, guarantees that simultaneously its brightness, whiteness, form and aspect, pH are not affected, and more can be applicable to chemical fibre industry; The resistivity of gained white titanium pigment is 2800-3600 Ω cm, pH 6.5-7.5, brightness Δ L>=99.50, Δ b (being form and aspect)≤0.5;
2, technology of the present invention is compared with the salt treatment agent addition of prior art, produces cost-saved 51 yuan of 1 ton of titanium white (all by intermediate value);
To sum up, working method of the present invention is simple, and on-the-spot technical process does not need to transform, and feasibility is strong.
Embodiment
The invention provides a kind of method of producing the high resistivity white titanium pigment, concrete steps are:
The preparation of A titanium liquid
With obtaining titanium liquid behind titanium slag and titanium ore and the sulfuric acid reaction, to the dense titanium liquid that meets the hydrolysis requirement, the specific targets of dense titanium liquid are as shown in table 1 with the allotment of titanium liquid water:
The dense titanium liquid of table 1 index
Annotate: the stability in the table (ml/ml), front " ml " represents the zero(ppm) water consumption, and " ml " is the dense titanium liquid of 1ml at the back.
The hydrolysis of B titanium liquid
Hydrolyzing process of the present invention is consistent with existing plus seed ordinary-pressure hydrolysis; Promptly after titanium liquid preheating → preparation crystal seed → hydrolysis, can obtain metatitanic acid; (D represents the diameter of powder granule to particle diameter D50; D50 representes the diameter of 50% of accumulative total, or claims 50% through particle diameter, and D50 claims median size or meso-position radius again) be controlled between the 1.5 μ m-1.7 μ m.Because the concentration of metatitanic acid slurry need be controlled at 300-340g/l in the follow-up salt treatment step; If particle diameter surpasses 1.7 μ m; It is too much then can to cause slurry to add shallow de-mineralized water, thereby the salt treatment agent can dissolve in the shallow de-mineralized water in a large number, before kiln in the pressure-filtering process; Can cause the salt treatment agent to run off in a large number, thereby influence the titanium white quality; If the hydrolysis particle diameter is lower than 1.5 μ m, the particle specific surface area is excessive, and slurry concentration is controlled at 300-340g/l in the salt treatment step, and it is very few then can to cause slurry to add shallow de-mineralized water, the salt treatment agent can not be in slurry homodisperse, thereby influence the salt treatment effect.
C washing, rinsing
The metatitanic acid slurry of hydrolysis gained is used water washing after removing by filter adsorbed mother liquor, its acid filtrate should reclaim or handle the back discharging; Wash later metatitanic acid and under acid and reductive condition, bleach earlier, post rinse is removed remaining impurity iron.
The salt of D metatitanic acid is handled
(1) the metatitanic acid slurry after the rinsing is squeezed into salt and handle pot, add shallow de-mineralized water and regulate the metatitanic acid slurry concentration, make it be controlled at 300-340g/l; If the metatitanic acid slurry concentration is lower than 300g/l, sylvite can run off in a large number when follow-up filter-press dehydration, thereby the salt treatment agent that remains in the metatitanic acid is very few, causes resistivity higher; If the metatitanic acid slurry concentration is higher than 340g/l, material viscosity is bigger, and sylvite disperses inhomogeneous, thereby can cause the fluctuation of titanium white finished product resistivity bigger; Wherein, the preparation method of shallow de-mineralized water is: with the Ca in the cationic exchange resin adsorption tap water
2+, Mg
2+, Na
+Deng just making shallow de-mineralized water behind the positively charged ion, shallow de-mineralized water is slightly acidic, pH 2-3;
(2) salt is handled: after the slurry after the rinsing is squeezed into salt and handled pot and stir 30min, add and contain the potassium material and stir 30min, the add-on that contains the potassium material is that the 0.39-0.47wt% of titanium oxide (in the content of titanium dioxide in the metatitanic acid) is (with K
2The O meter); Add phosphoric acid again and stir 30min, the add-on of phosphoric acid is that the 0.28-0.30wt% of titanium oxide is (with P
2O
5Meter); Salt handle the metatitanic acid slurry, be put into storage tank before the kiln; The adding that contains the potassium material can be controlled at 2800-3600 Ω cm with resistivity, and the titanium white resistivity that relates in the literary composition is poach resistivity; The adding of phosphoric acid can make the pH value be controlled between the 6.5-7.5, effect that also can hidden impurity element iron.Add the salt treatment agent and can also play following effect: 1. make metatitanic acid desulfurization at a lower temperature, reduce calcining temperature and make material reach neutral at a lower temperature; 2. promote TiO
2The growth of microcrystal; 3. improve pigment performance, make that the white titanium pigment particle is soft, color and luster is pure white, reducing power improves.Add earlier during salt is handled and contain the potassium material, the reason that adds phosphoric acid again is: for making the effect of its hidden impurity element iron of phosphoric acid performance, just must guarantee that phosphoric acid fully reacts with the ironic hydroxide in the metatitanic acid; And mostly the potassium material is alkalescence, and phosphoric acid is tart, adds simultaneously and will react to each other, and causes effect to decrease.In fact, contain potassium material and phosphoric acid and add simultaneously salt handled and be free from side effects, the amount that just adds phosphoric acid just should be carried out suitable adjustment, thereby has increased cost.
The calcining of E metatitanic acid slurry
Carry out processed to the metatitanic acid slurry after the salt processing, control metatitanic acid water cut is 37-47wt%; Because sylvite is water-soluble, therefore come the controlling resistance rate through residual sylvite amount in the control metatitanic acid, if water cut is lower than 37%, then residual sylvite amount is less in the metatitanic acid, thus resistivity surpasses 3600 Ω cm; If water cut is higher than 47%, then residual sylvite amount is higher in the metatitanic acid, and resistivity can not reach 2800 Ω cm on the one hand; On the other hand, because water cut is excessive, rotary kiln dehydration difficulty during calcining, kiln end temperature is low, and vent gas treatment also increases burden.The calcining powder process in rotary kiln of dehydration back promptly gets white titanium pigment; Wherein, the calcining process parameter is: kiln speed (branch/commentaries on classics)/4-4.5, temperature of kiln head/880-905 ℃, kiln end temperature/290-320 ℃.
The chemical fibre field decides through consultation that with white titanium pigment the performance index of appearance are generally: resistivity 2800-3600 Ω cm, pH 6.5-7.5, brightness (Δ L)>=99.50, Δ b (being form and aspect)≤0.5.
Do further description below in conjunction with the embodiment specific embodiments of the invention, therefore do not limit the present invention among the described scope of embodiments.
Material and equipment:
1, material: dense titanium liquid, Pottasium Hydroxide, phosphoric acid, shallow de-mineralized water.
2, equipment: hydrolyzer (volume: 110m
3), salt is handled pot (volume: 16m
3), diaphragm filter press (area: 450m
2), rotary kiln (outside diameter 2.8m, long 55m).
Embodiment 1
(1) dense titanium liquid index is seen table 2;
The dense titanium liquid of table 2 index
(2) hydrolyzing process is consistent with existing plus seed ordinary-pressure hydrolysis, promptly after titanium liquid preheating → preparation crystal seed → hydrolysis, can obtain metatitanic acid, and particle diameter D50 is: 1.51 μ m;
(3) slurry after the rinsing is squeezed into salt and handle pot, add shallow de-mineralized water and regulate the dense 328g/l of being of metatitanic acid slurry;
(4) after slurry stirs 30min, add Pottasium Hydroxide, the add-on of Pottasium Hydroxide is the 0.46wt% of content of titanium dioxide (in the content of titanium dioxide in the metatitanic acid); Stir 30min; The phosphoric acid that adds the 0.28wt% of content of titanium dioxide again stirs 30min, and blowing is to the preceding storage tank of kiln;
(5) pump into diaphragm filter press to slurry through press filtration 0.5h, water cut is 40%;
(6) calcined by rotary kiln powder process, the calcining process parameter is: kiln speed (branch/commentaries on classics)/4.25, temperature of kiln head/902 ℃, kiln end temperature/305 ℃, production capacity (ton/sky)/51.
(7) finished product after will pulverizing carries out the optical property index determining, and the result sees table 4.
Embodiment 2
Different among the add-on of removing Pottasium Hydroxide in the step (4) and the embodiment 1, other steps are all with embodiment 1, and the add-on of the middle Pottasium Hydroxide of step (4) is the 0.41wt% of content of titanium dioxide; The products obtained therefrom performance is as shown in table 4.
Comparative Examples 1
(1) dense titanium liquid parameter is seen table 3;
The dense titanium liquid of table 3 index
(2) hydrolyzing process is consistent with existing plus seed ordinary-pressure hydrolysis, promptly after titanium liquid preheating → preparation crystal seed → hydrolysis, can obtain metatitanic acid, and particle diameter D50 is: 1.55 μ m;
(3) slurry after the rinsing is squeezed into salt and handle pot, add shallow de-mineralized water and regulate the dense 330g/l of being of metatitanic acid slurry;
(4) behind the slurry stirring 30min, add Pottasium Hydroxide, the add-on of Pottasium Hydroxide is the 0.60wt% of content of titanium dioxide, stirs 30min, adds the phosphoric acid that accounts for titanium oxide 0.25wt% again and stirs 60min, and blowing is to the preceding storage tank of kiln;
(5) pump into diaphragm filter press to slurry through press filtration 0.5h, water content 39%;
(6) calcined by rotary kiln powder process, the calcining process parameter is: kiln speed (branch/commentaries on classics)/4.25, temperature of kiln head/900 ℃, kiln end temperature/300 ℃, production capacity (ton/sky)/50.
(7) finished product after will pulverizing carries out the optical property index determining, and the result sees table 4.
Comparative Examples 2
The add-on of removing Pottasium Hydroxide in the step (4) is different with embodiment 1, and other steps are all with embodiment 1, and the add-on of Pottasium Hydroxide accounts for the 0.39wt% of content of titanium dioxide in the step (4); Gained PERFORMANCE OF TITANIUM DIOXIDE PIGMENT index is as shown in table 4.
Comparative Examples 3
The add-on of removing Pottasium Hydroxide in the step (4) is different with embodiment 1, and other steps are all with embodiment 1, and the add-on of Pottasium Hydroxide accounts for the 0.48wt% of content of titanium dioxide in the step (4); Gained PERFORMANCE OF TITANIUM DIOXIDE PIGMENT index is as shown in table 4.
Comparative Examples 4
The add-on of removing Pottasium Hydroxide in the step (4) is different with embodiment 1, and other steps are all with embodiment 1, and the add-on of Pottasium Hydroxide accounts for the 0.38wt% of content of titanium dioxide in the step (4); Gained PERFORMANCE OF TITANIUM DIOXIDE PIGMENT index is as shown in table 4.It is thus clear that when the add-on of Pottasium Hydroxide was the 0.38wt% of content of titanium dioxide, though the resistivity of gained white titanium pigment is higher, its form and aspect and whiteness value obviously can not reach request for utilization.In the white titanium pigment field, product is compared its brightness Δ L>=99.50 with deciding through consultation standard specimen, and Δ b≤0.5 shows that the whiteness of this sample, form and aspect meet request for utilization.
Table 4 white titanium pigment target level of product quality
In the table 4, L is a brightness value; A representes form and aspect, and a >=0 o'clock is red phase, and a＜0 is green phase; B representes form and aspect, and b >=0 o'clock is yellow phase, and b＜0 is blue phase; Δ L: sample brightness value * 100/ standard specimen brightness value; Δ b:| sample hue value-standard specimen hue value |.
The standard specimen that adopts in the embodiment of the invention is the commodity of another name for Sichuan Province, Yunnan, Shanghai chemical industry ltd.Can know by last table; The white titanium pigment product that utilizes the inventive method to obtain is close basically with brightness, whiteness, form and aspect, the pH numerical value of the white titanium pigment sample that adopts existing sulfuric acid process to produce; All can satisfy request for utilization; And that the present invention obtains the resistivity MV of white titanium pigment product is higher, the highlyest exceeds 900 Ω cm.It is thus clear that, adopt method of the present invention to prepare white titanium pigment, guaranteeing that its resistivity is higher under the qualified situation of performances such as product brightness, whiteness, form and aspect, be suitable for chemical fibre industry.
Claims (7)
1. the working method of high resistivity white titanium pigment adopts the sulfuric acid method titanium pigment production technique, comprises the steps: that hydrolysis, washing, the salt of titanium liquid is handled, calcining powder process, wherein:
Add in the salt treatment step and contain the potassium material, the add-on that contains the potassium material accounts for the 0.39-0.47wt% of content of titanium dioxide, and wherein, containing the potassium material is potassic alkali or salt.
2. the working method of high resistivity white titanium pigment according to claim 1 is characterized in that: the said potassium material that contains is at least a in Pottasium Hydroxide, vitriolate of tartar, salt of wormwood, the potassiumphosphate.
3. the working method of high resistivity white titanium pigment according to claim 1 and 2 is characterized in that: add phosphoric acid in the salt treatment step, the add-on of phosphoric acid accounts for the 0.28-0.3wt% of content of titanium dioxide.
4. according to the working method of each described high resistivity white titanium pigment of claim 1-3, it is characterized in that: in the hydrolysing step of titanium liquid, get the metatitanic acid slurry after the hydrolysis, the median size of metatitanic acid is controlled at 1.5 μ m-1.7 μ m.
5. according to the working method of each described high resistivity white titanium pigment of claim 1-4, it is characterized in that: in the salt treatment step, regulating the metatitanic acid slurry concentration is 300-340g/l.
6. the working method of high resistivity white titanium pigment according to claim 5 is characterized in that: in the salt treatment step, add earlier and contain the potassium material, add phosphoric acid again.
7. according to the working method of each described high resistivity white titanium pigment of claim 1-6, it is characterized in that: in the calcining powder process step, the metatitanic acid slurry after salt is handled carries out processed, makes its water cut be controlled to be 37-47wt%.
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Cited By (7)
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| CN103043715A (en) * | 2012-12-19 | 2013-04-17 | 攀枝花鼎星钛业有限公司 | Production method of titanium dioxide powder |
| CN103241770A (en) * | 2013-05-22 | 2013-08-14 | 河南佰利联化学股份有限公司 | Meta titanate treatment method |
| CN104477989A (en) * | 2014-10-24 | 2015-04-01 | 宁波新福钛白粉有限公司 | Preparation method of titanium dioxide for printing ink |
| CN105152210A (en) * | 2015-10-23 | 2015-12-16 | 云南千盛实业有限公司 | Substitution reaction method of titanium dioxide |
| CN106853994A (en) * | 2015-12-09 | 2017-06-16 | 攀枝花市钛都化工有限公司 | Titanium dioxide combines salt accelerator |
| CN115924966A (en) * | 2022-12-12 | 2023-04-07 | 龙佰四川钛业有限公司 | Titanium white powder salt treating agent recovery process and titanium white powder production process |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102963927A (en) * | 2012-12-14 | 2013-03-13 | 中国有色集团（广西）平桂飞碟股份有限公司 | Method for pretreating titanium dioxide before sintering |
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| CN104477989A (en) * | 2014-10-24 | 2015-04-01 | 宁波新福钛白粉有限公司 | Preparation method of titanium dioxide for printing ink |
| CN105152210A (en) * | 2015-10-23 | 2015-12-16 | 云南千盛实业有限公司 | Substitution reaction method of titanium dioxide |
| CN106853994A (en) * | 2015-12-09 | 2017-06-16 | 攀枝花市钛都化工有限公司 | Titanium dioxide combines salt accelerator |
| CN115924966A (en) * | 2022-12-12 | 2023-04-07 | 龙佰四川钛业有限公司 | Titanium white powder salt treating agent recovery process and titanium white powder production process |
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