CN108946806A - A kind of production method of high covering power titanium dioxide - Google Patents
A kind of production method of high covering power titanium dioxide Download PDFInfo
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- CN108946806A CN108946806A CN201811034132.0A CN201811034132A CN108946806A CN 108946806 A CN108946806 A CN 108946806A CN 201811034132 A CN201811034132 A CN 201811034132A CN 108946806 A CN108946806 A CN 108946806A
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- titanium dioxide
- covering power
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/08—Drying; Calcining ; After treatment of titanium oxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention relates to titanium dioxide preparation fields, more particularly to a kind of production method of high covering power titanium dioxide, mainly comprise the steps that (1) raw ore crushes, (2) acidolysis, (3) it leaches, (4) it restores, (5) it settles, (6) concentration of titanium liquid, (7) it hydrolyzes, (8) it washes and bleaches, (9) salt treatment, (10) it filters, calcining, surface treatment, (11) dry, dedusting, it is characterized by: the calcining seeds for being equivalent to the 2.0-3.0% of TiO2 content are added in meta-titanium acid solution into the bleaching process of step (8), calcination temperature is 700-960 DEG C.The present invention is in experimental basis largely, repeatedly, continuous summing up experience, improvement are perfect, it is determined that high covering power titanium white production method as described in the present invention passes through the content for reducing calcining seeds, regulate and control the temperature in calcination process, to achieve the purpose that improve titanium dioxide covering power.
Description
Technical field
The present invention relates to the production technical field of titanium dioxide, especially a kind of high production method for covering titanium dioxide.
Background technique
Titanium dioxide pigment is best white pigment, it has, and whiteness is high, opacity is high, physicochemical properties are stablized
The advantages that, it is widely used in the industries such as coating, plastics, papermaking.The titanium dioxide of high covering power can not only be such that its application system obtains
Splendid opacity is obtained, and can reduce manufacturing cost, therefore, for titanium dioxide user, covering power is both one
Technical indicator and an economic indicator.
In coating application field, the covering power and pigment of titanium dioxide and the difference of resin index are related, and difference is bigger, cover
Power is higher.Since the refractive index of hydrated SiO 2 is minimum, hydrated SiO 2 is introduced in the surface treatment process of titanium dioxide
This refractive index difference can be increased, single titanium dioxide particle can also be made to the maximum extent by coating a large amount of hydrated SiO 2
Isolation between each other is in good dispersity, to significantly improve the utilization rate of titanium dioxide.Additionally, due to the refraction of air
Rate be it is minimum in all substances, in building coating, due to formula in pigment volumetric concentration it is higher, the volume of pigment is dense
After degree is greater than critical size concentration, resin in film cannot coated pigment particle completely, to make empty containing part in film
Gas can significantly improve film to the covering power of building matrix since the refraction difference of pigment and air is maximum；If
One layer of loose coating layer is introduced in the surface treatment of titanium dioxide, and the air capacity in film can be improved, reach raising titanium dioxide
The purpose of covering power.
Using the hydrate of a large amount of silica-alumina of cladding on the surface of titanium dioxide to improve it in paint field
Covering power is a kind of technology being widely used, such as United States Patent (USP) US3437502, US3510335, US4075031 etc..
United States Patent (USP) US3437502 discloses a kind of production method of improved titanium dioxide pigment, by titanium dioxide
Compact silicon dioxide and one layer of one layer of the titanium particle surface cladding based on titanium dioxide quality 0.5~25% are based on titanium dioxide matter
The aluminium oxide of amount 0.1~10%, to obtain a kind of dioxy of good dispersion with high covering power and in aqueous coating formulation
Change titanium pigment, the coating using the titanium white production of this method preparation has excellent outdoor weathe resistance.
United States Patent (USP) US3510335 disclose it is a kind of coat about 1 in titania-alumina cooxidation object surface of pigments~
Then 25% porosity and looseness silicon dioxide film is calcined under the conditions of 300~1000 DEG C, obtain a kind of fastness and high covering power titanium
White powder.
United States Patent (USP) US4075031 discloses a kind of method for improving titanium dioxide pigment covering power, by titanium dioxide
Surface of pigments coats one layer of fine and close amorphous silica and pellumina, then coats one layer of porous silica-alumina
Film, to ensure that the weatherability of titanium dioxide while improving covering power.
In short, no matter using cladding process or the method for calcining preceding salt treatment, the titanium white of all not getable high covering power
Powder.
Summary of the invention
The main object of the present invention is in view of the above shortcomings of the prior art, to provide a kind of a kind of new high covering titanium dioxide
Production method improve calcination temperature, guarantee the golden red in the case of low crystal seed dosage by adjusting LR-952 calcining seeds dosage
Stone conversion ratio improves the seed sized in conversion process, achievees the purpose that improve product covering power.
Calcining seeds have reduce titanium dioxide phase transition temperature, adjust rutile titanium dioxide grain size and from
The effect of sub- pattern, additional amount increase, and the titania fired is tiny, and particle shape is more mellow and full, covering power meeting
Increase, but when calcining seeds additional amount is excessive, just there is no obvious effect for the raising contribution of covering power；And metatitanic acid is forged
Temperature increases during burning, and covering power also will increase, but temperature improves too much, and will cause TiO 2 particles excess agglomeration,
Covering power can decline again, and therefore, the present invention is high to obtain using the adding proportion and adjustment calcination temperature of allotment calcining seeds
Covering power.
In order to achieve the above-mentioned object of the invention, The technical solution adopted by the invention is as follows:
A kind of production method of high covering power titanium dioxide, is prepared by the following steps to obtain:
(1) raw ore crushes, (2) acidolysis, (3) leaching, (4) reduction, (5) sedimentation, the concentration of (6) titanium liquid, (7) hydrolysis, (8) washing
And bleaching, (9) salt treatment, (10) filtering, calcining, surface treatment, (11) drying, dedusting, it is characterised in that: to step (8)
The calcining seeds for being equivalent to the 2.0-3.0% of TiO2 content, calcination temperature 700- are added in meta-titanium acid solution in bleaching process
960℃。
Preferably, the additional amount of calcining seeds is 2.9%, 2.6%, 2.3%；
Preferably, calcination temperature is 750 DEG C, 800 DEG C, 850 DEG C, 900 DEG C, 950 DEG C.
Salt treatment process step is specific as follows: step 1, and the calcining gold of 2.0-3.0% is added in the meta-titanium acid solution after bleaching
Red stone-type crystal seed；ZnO, NH4H2PO4, KOH, Al2 (SO4) 3 is added in step 2.With being pumped into kiln tail storage tank.But above-mentioned five
Substance additional proportion needs strict control.
Wherein, above-mentioned salt treatment it is specific with rutilization nuclei the preparation method is as follows:
A. the preparation of positive sodium titanate: the TiO2 hydrate that filter press filtration washing qualification iron content is lower than 50ppm is washed through two, with pump
Be sent to metatitanic acid heating measuring tank, NaOH through alkali heating measuring tank metering after be heated separately to 60 DEG C and 90 DEG C after, by TiO2 water
It closes object NaOH and is put into alkali fusion tank and carry out reaction and 50%NaOH solution reaction, generate positive sodium titanate.It is beaten after cooling with pump
Enter filter press by upper piece, washing, discharging, filter cake mashing, positive sodium titanate from contain a large amount of free NaOH solution filtrate in
It separates, 15%NaOH filtrate flows into ammonium hydroxide collecting tank, then is used as tail gas spray with pumping external system.It is washed just with filter press
NaOH in sodium titanate filter cake, after measuring filtrate NaOH content less than 1500ppm, discharging enters hollander tub, then again with 10%
Hydrochloric acid is neutralized to pH value in 3.5~4.0 ranges, with pump squeeze into filter press using upper piece, washing, until washing filtrate pH value is big
When 7, the control of TiO2 concentration is made in 200~220g/l, for producing among the positive metatitanic acid of crystal seed preparation in discharging, filter cake mashing
Product.B. prepared by crystal seed: the positive sodium titanate of step A is reacted with 30% hydrochloric acid generates rutile type calcining seeds, makes
Crystal seed pump is squeezed into storage tank.
The utility model has the advantages that the present invention, in experimental basis largely, repeatedly, continuous summing up experience, improvement are perfect, it is determined that such as
High covering power titanium white production method of the present invention regulates and controls the temperature in calcination process by reducing the content of calcining seeds
Degree, to achieve the purpose that improve titanium dioxide covering power.
Specific embodiment
The present invention is described in further detail With reference to embodiment.
But the range that this should not be interpreted as to the above-mentioned theme of the present invention is only limitted to following embodiments.On not departing from the present invention
In the case of stating technical idea, according to ordinary skill knowledge and customary means, various replacements and change are made, should all include
Within the scope of the invention.
Embodiment 1
The present embodiment method for producing rutile type titanium white powder with high hiding power includes the following steps:
(1) prepare metatitanic acid slurry: take one wash after metatitanic acid, enough deionized waters are added, are configured to slurry gross mass
For 1500g, the metatitanic acid slurry that TiO2 content is 25%；
(2) bleaching of metatitanic acid: it is slowly added to 90g, 98% concentrated sulfuric acid into metatitanic acid slurry, and is stirred, then by body
System is heated to 60 DEG C in a water bath；
(3) 2.3% calcining seeds for being equivalent to TiO2 content are added into above-mentioned slurry, 12g mass point is added after stirring 30min
The Ti3+ solution that number is 5.15% then proceedes to stirring 90min；
(4) with temperature be 50-80 DEG C deionized water detergent bleach after metatitanic acid, then mashing is configured to the inclined titanium of 300g/L
Wintercherry material simultaneously carries out quantitative analysis to slurry ferrous iron, controls within 20ppm range；
(5) it is its additional amount of 17.31% KOH(in terms of K2O mass that 5.84g mass fraction is added into above-mentioned slurry, accounts for dioxy
Change the 0.27% of titanium quality)；
(6) it is its additional amount of 23.86% H3PO4(in terms of P2O5 mass that 3.14g mass fraction, which is added, accounts for titanium dioxide quality
0.20%)；
(7) it is its additional amount of 5.64% Al2 (SO4) 3(in terms of Al2O3 mass that 17.95g mass fraction, which is added, accounts for titanium dioxide
The 0.27% of quality)；
(8) it is its additional amount of 1.0% MgSO4(in terms of MgO mass that 56.25g mass fraction, which is added, accounts for titanium dioxide quality
0.15%)；
(9) 700 DEG C will be raised to from room temperature in one hour in Muffle furnace after the drying of above-mentioned slurry, be then heated up with 1 DEG C/min fast
Degree is warming up to 950 DEG C from 700 DEG C up to rutile titanium dioxide substrate.
Comparative example
Step corresponds to embodiment 1, and only having adjusted calcining seeds content is 5%, and calcination temperature is within the scope of 990 DEG C.
As it can be seen from table 1 using titanium dioxide substrate made from the method for the present invention covering power compared with comparative example obtained compared with
It increases substantially, there is potential application foreground in the coating and ink area of high PVC concentration.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (4)
1. a kind of production method of high covering power titanium dioxide, mainly comprises the steps that
(1) raw ore crushes, (2) acidolysis, (3) leaching, (4) reduction, (5) sedimentation, the concentration of (6) titanium liquid, (7) hydrolysis, (8) washing
And bleaching, (9) salt treatment, (10) filtering, calcining, surface treatment, (11) drying, dedusting, it is characterised in that: to step (8)
The calcining seeds for being equivalent to the 2.0-3.0% of TiO2 content, calcination temperature 700- are added in meta-titanium acid solution in bleaching process
960℃。
2. a kind of production method of high covering power titanium dioxide as described in claim 1, it is characterised in that: the addition of calcining seeds
Amount is 2.9%, 2.6%, 2.3%.
3. a kind of production method of high covering power titanium dioxide as described in claim 1, it is characterised in that: calcination temperature 750
℃、800℃、850℃、900℃、950℃。
4. a kind of production method of high covering power titanium dioxide as described in claim 1, which is characterized in that salt treatment process step
Specific as follows: the calcining rutilization nuclei of 2.0-3.0% is added in step 1, the meta-titanium acid solution after bleaching；Step 2 is added
ZnO、H2PO4、 KOH、Al2(SO4)3。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112499677A (en) * | 2020-12-17 | 2021-03-16 | 襄阳龙蟒钛业有限公司 | Method for improving activity of calcined seed crystal |
| CN113549345A (en) * | 2021-08-26 | 2021-10-26 | 苏州市宏丰钛业有限公司 | Preparation method and system of titanium dioxide for plastics |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112499677A (en) * | 2020-12-17 | 2021-03-16 | 襄阳龙蟒钛业有限公司 | Method for improving activity of calcined seed crystal |
| CN113549345A (en) * | 2021-08-26 | 2021-10-26 | 苏州市宏丰钛业有限公司 | Preparation method and system of titanium dioxide for plastics |
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