CN101844803A - Rutile type titanium dioxide and preparation method thereof - Google Patents
Rutile type titanium dioxide and preparation method thereof Download PDFInfo
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- CN101844803A CN101844803A CN200910106449A CN200910106449A CN101844803A CN 101844803 A CN101844803 A CN 101844803A CN 200910106449 A CN200910106449 A CN 200910106449A CN 200910106449 A CN200910106449 A CN 200910106449A CN 101844803 A CN101844803 A CN 101844803A
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Abstract
The invention provides a rutile type titanium dioxide and a preparation method thereof, wherein the rutile type titanium dioxide contains zinc compound and lithium compound. The preparation method of the rutile type titanium dioxide comprises that the compound containing anatase titanium dioxide, rutile type titanium dioxide seed crystal and lithium salt is calcinated to obtain the rutile type titanium dioxide; and the method for preparing the rutile type titanium dioxide seed crystal comprises that: in the presence of water, metatitanic acid is contacted with zinc salt, and the contact temperature is 40-80 DEG C. By adopting the method provided by the invention, the conversion rate of the rutile type titanium dioxide reaches above 98%. In addition, the preparation method of the rutile type titanium dioxide of the invention is simple, and has less process and low cost.
Description
Technical field
The present invention relates to the titanium dioxide field, particularly a kind of rutile titanium dioxide and preparation method thereof.
Background technology
Titanium dioxide (titanium dioxide) is because of having superior whiteness, tinting strength, opacifying power, weathering resistance, thermotolerance and chemical stability, and do not have toxicity, is widely used in fields such as coating, plastics, papermaking, printing ink and chemical fibre.The wider titanium dioxide of present industrial application is that anatase titanium dioxide (Anatase) is called for short the A type, and rutile-type (Rutile) is called for short the R type.Because the anatase thpe white powder cost of investment is relatively low, product processes is simple, and domestic most of titanium white production producer is to produce anatase thpe white powder.But with respect to anatase thpe white powder, Rutile type Titanium Dioxide has the specific refractory power height, and opacifying power is good, compact structure, and hardness, density are bigger, and photochemical activity is little, advantage such as weather resistance, weathering resistance are good.Yet the technological process of production of Rutile type Titanium Dioxide is long in the prior art, and technology is very accurate complicated, the production cost height.
Prior art discloses a kind of method that iron protochloride prepares Rutile type Titanium Dioxide of introducing, and this method mainly may further comprise the steps: the ilmenite sulfuric acid solution obtains titanyl sulfate solution, and after deironing purified, (consumption was TiO to introduce solution of ferrous chloride
2: FeCl
2.4H
2O=1: 0.97~3.88), the freezing ferrous sulfate of removing adds the crystal seeds of rutile of 1-6% then, heating hydrolysis, metatitanic acid washing, removal of impurities, rinsing, drying, grinding with gained count crystal type promoting reagent ZnO and MgO again, calcine 6-10 hour down for 750-850 ℃.This method adopts ZnO and MgO as crystal type promoting reagent, but this method calcining temperature is higher, needs soaking time longer, and therefore production cost is higher in actual production process, and production efficiency is lower; And rutile titanium white powder rate transition that this method is produced is not high, and is generally below 95%, therefore bigger to the final product quality influence.
In addition, prior art also discloses a kind of method of microwave heating method for preparing rutile type titanium white, and this method discloses a kind of microwave radiation micro-wave dielectric heat effect after the match of utilizing, and makes anatase thpe white powder transform into the method for Rutile type Titanium Dioxide.But this method production unit requires high, and preparation method's complexity and transformation efficiency are not high.
Summary of the invention
The objective of the invention is provides a kind of rutile titanium dioxide and preparation method thereof in order to overcome the low shortcoming of preparation method's complexity, transformation efficiency of rutile titanium dioxide in the prior art.
The invention provides a kind of rutile titanium dioxide, contain zn cpds and lithium compound in the described rutile titanium dioxide.
The present invention also provides a kind of preparation method of rutile titanium dioxide, and wherein, this method comprises that the mixture roasting that will contain anatase titanium dioxide, rutile titanium dioxide crystal seed and lithium salts obtains rutile titanium dioxide; The described method for preparing the rutile titanium dioxide crystal seed comprises: in the presence of water, metatitanic acid is contacted with zinc salt, the temperature of contact is 40-80 ℃.
The transformation efficiency that adopts rutile crystal type promotor provided by the present invention to prepare rutile titanium dioxide reaches more than 98%.In addition, the preparation method of rutile titanium dioxide of the present invention is easy, operation is few, and cost is low.
Embodiment
The invention provides a kind of rutile titanium dioxide, contain zn cpds and lithium compound in the described rutile titanium dioxide.
According to rutile titanium dioxide provided by the invention, in the described rutile titanium dioxide, with Li
+Meter, the content of described lithium compound accounts for the 0.1-1 quality % of rutile titanium dioxide, is preferably 0.2-0.6 quality %; With Zn
2+Meter, the content of described zn cpds accounts for the 0.1-0.8 quality % of rutile titanium dioxide, is preferably 0.3-0.6 quality %.
The present inventor thinks that described lithium compound is dispersed in the rutile titania powder with the form of Lithium Oxide 98min, perhaps is entrained in the titanium dioxide crystal lattice with the lithium atom attitude; Similarly, described zn cpds is dispersed in the rutile titania powder with the form of zinc oxide, perhaps is entrained in the titanium dioxide crystal lattice with the zinc atom attitude.
Under the preferable case, also contain at least a in magnesium compound, the tin compound in the described rutile titanium dioxide.Further, in the described rutile titanium dioxide, the content of magnesium compound accounts for the 0.1-1.2 quality % of rutile titanium dioxide, is preferably 0.2-0.8 quality %; The content of tin compound accounts for the 0.03-0.3 quality % of rutile titanium dioxide, is preferably 0.05-0.18 quality %.
The present invention also provides a kind of preparation method of rutile titanium dioxide, and this method comprises that the mixture roasting that will contain anatase titanium dioxide, rutile titanium dioxide crystal seed and lithium salts obtains rutile titanium dioxide; The described method for preparing the rutile titanium dioxide crystal seed comprises: in the presence of water, metatitanic acid is contacted with zinc salt, the temperature of contact is 40-80 ℃.
Designer of the present invention finds by a large amount of experiments, adopts lithium salts can improve the transformation efficiency of anatase titanium dioxide to rutile titanium dioxide during the preparation rutile titanium dioxide.When high-temperature roasting, the lithium ion in the lithium salts can infiltrate in the lattice of anatase titanium dioxide when high temperature fast as leading brilliant ion, promotes the fast transition of anatase titanium dioxide to rutile titanium dioxide, shortens the reaction times, increases transformation efficiency.Described lithium salts can be in Lithium Sulphate, lithium nitrate and the Quilonum Retard one or more.
As long as be used to prepare the amount of the water of described crystal seed described metatitanic acid and zinc salt are fully disperseed, what of the amount of described water are little to the influence that realizes purpose of the present invention, and therefore, the consumption of described water can change in the larger context.Under the preferable case, be benchmark with the metatitanic acid of 100 weight parts, the consumption of described zinc salt is the 1-10 weight part, and the consumption of water is the 100-250 weight part.
According to method provided by the present invention, the time of described contact is 30-150 minute.Under the preferable case, described contact is divided into two stages, and the temperature of two stage contacts is 40-80 ℃, and the time of contact is respectively 30-70 minute and 20-60 minute, and also comprises the pH to 4-5 that regulates this mixture with acid between two stages.Described acid can various acid, as long as can regulate the pH value to required scope.For example, described acid can be one or more in sulfuric acid, hydrochloric acid and the nitric acid.
Described zinc salt can be various zinc salts, all can realize purpose of the present invention, and under the preferable case, described zinc salt is one or more in zinc oxide, zinc carbonate, zinc chloride, zinc sulfate, the zinc nitrate.
As long as contain rutile titanium dioxide crystal seed and lithium salts in the described mixture, just anatase titanium dioxide can be converted into rutile titanium dioxide, the consumption of described rutile titanium dioxide crystal seed and lithium salts can change in the larger context.Consider the foreign matter content in the product that finally obtains and the transformation efficiency of rutile titanium dioxide, under the preferable case, be benchmark with the anatase titanium dioxide of 100 weight parts, with dry weight basis, the consumption of described rutile titanium dioxide crystal seed is the 5-15 weight part, is preferably the 8-12 weight part; The consumption of described lithium salts is the 0.3-3 weight part, is preferably the 0.5-2 weight part.Need to prove that dry weight of the present invention is meant that the crystal seed that will be made by method of the present invention removes the weight of anhydrating to constant weight under 1 normal atmosphere, 100 ℃ under nitrogen atmosphere.
According to method provided by the present invention, can also contain carbonate in the described mixture.Carbanion in the carbonate can produce titanium dioxide gas in roasting process, make the Rutile type Titanium Dioxide that makes comparatively loose.Described carbonate can be in lime carbonate, the magnesiumcarbonate at least a.
More preferably under the situation, according to method provided by the present invention, be benchmark with the anatase titanium dioxide of 100 weight parts, with dry weight basis, the consumption of described carbonate is the 0.5-4 weight part.
As a preferred embodiment of the present invention, contain Quilonum Retard in the described mixture; During high-temperature roasting, Quilonum Retard can provide lithium ion as lithium salts, can provide carbanion as carbonate again, can effectively improve the transformation efficiency of rutile titanium dioxide, and the rutile titanium dioxide that obtains is loose, can also effectively reduce the content of impurity in the rutile titanium dioxide simultaneously.
The preparation method of rutile titanium dioxide provided by the present invention, can also contain metal oxide in the described mixture, the various metal oxides that described metal oxide is used always for those skilled in the art for example can be in magnesium oxide, zinc oxide and the tindioxide one or more.
Under the preferable case,, effectively reduce calcining temperature simultaneously in order to improve the transformation efficiency of rutile titanium dioxide, shortening soaking time, is benchmark with the anatase titanium dioxide of 100 weight parts, with dry weight basis, described magnesian consumption is the 0.2-3 weight part, more preferably the 0.5-2 weight part; The consumption of described zinc oxide is the 0.2-2.5 weight part, more preferably the 0.4-1.8 weight part; The consumption of described tindioxide is the 0.02-0.2 weight part, more preferably the 0.05-0.15 weight part.
The temperature and time of described roasting can change in the larger context, all can realize purpose of the present invention.From time and cost consideration, the temperature of described roasting is preferably 700-900 ℃, and the time of roasting is preferably 1-5 hour, more preferably 1-2 hour.In addition, preferably before carrying out described roasting, earlier described mixture is carried out preheating, the temperature of described preheating can be 200-400 ℃, and the time can be 10-30 minute.
In addition, described metatitanic acid and anatase titanium dioxide can prepare, and also can be commercially available.
In addition, method of the present invention also comprises the cooling of the product after the roasting, pulverizes.
Further specify the present invention below by embodiment.
Embodiment 1
Present embodiment illustrates the preparation method of rutile titanium dioxide of the present invention.
(1) preparation of crystal seed
The metatitanic acid, 1500 of 1000 grams is restrained water and 40 gram zinc oxide mixing stirrings, reacted 30 minutes down,, under 40 ℃, reacted 30 minutes then, make crystal seed with salt acid for adjusting pH value to 4 at 40 ℃.
(2) preparation of rutile titanium dioxide
With 1000 kilograms of anatase titanium dioxides (eastern good BA01-01 that Dong Jia company in Shandong produces, the scope of particle dia is 300-400nm) and 100 gram crystal seeds (with dry weight basis), 3.4 gram Quilonum Retard, 3.5 gram magnesium oxide, 0.1 gram tindioxide mixes, and the mixture that mixing is obtained is in muffle furnace, heated 10 minutes down at 200 ℃, be warmed up to 700 ℃ of insulations 2 hours then, cooling obtains product A 1.
(German LEO company LEO1450VP) measures the scope of product particle dia to adopt scanning electronic microscope; Measure the crystal formation and the transformation efficiency of product by X-ray diffractometer (Dutch Philips company, X ' PertPro).The result is as shown in table 1.
Embodiment 2
Present embodiment illustrates the preparation method of rutile titanium dioxide of the present invention.
(1) preparation of crystal seed
The metatitanic acid, 2500 of 1000 grams is restrained water and 100 gram zinc oxide mixing stirrings, reacted 30 minutes down,, under 70 ℃, reacted 20 minutes then, make crystal seed with salt acid for adjusting pH value to 5 at 70 ℃.
(2) preparation of rutile titanium dioxide
With 1000 kilograms of anatase titanium dioxides (eastern good BA01-01 that Dong Jia company in Shandong produces, the scope of particle dia is 300-400nm) and 150 gram crystal seeds (with dry weight basis), 9.9 gram Quilonum Retard, 6 gram magnesium oxide, 0.12 gram tindioxide mixes, and the mixture that mixing is obtained is in muffle furnace, heated 10 minutes down at 200 ℃, be warmed up to 900 ℃ of insulations 1.5 hours then, cooling obtains product A 2.
Measure scope, crystal formation and the particle diameter of the particle dia of product A 2 according to the method for embodiment 1.The result is as shown in table 1.
Embodiment 3
Present embodiment illustrates the preparation method of rutile titanium dioxide of the present invention.
(1) preparation of crystal seed
The metatitanic acid, 2400 of 1000 grams is restrained water and 50 gram zinc oxide mixing stirrings, reacted 40 minutes down,, under 40 ℃, reacted 60 minutes then, make crystal seed with salt acid for adjusting pH value to 4 at 50 ℃.
(2) preparation of rutile titanium dioxide
With 1000 kilograms of anatase titanium dioxides (eastern good BA01-01 that Dong Jia company in Shandong produces, the scope of particle dia is 300-400nm) and 100 gram crystal seeds (with dry weight basis), 10 gram Quilonum Retards mix, and the mixture that mixing is obtained is in muffle furnace, heated 10 minutes down at 200 ℃, be warmed up to 800 ℃ of insulations 2 hours then, cooling obtains product A 3.
Measure scope, crystal formation and the particle diameter of the particle dia of product A 3 according to the method for embodiment 1.The result is as shown in table 1.
Embodiment 4
Present embodiment illustrates the preparation method of rutile titanium dioxide of the present invention.
(1) preparation of crystal seed
The metatitanic acid, 2400 of 1000 grams is restrained water and 50 gram zinc oxide mixing stirrings, reacted 40 minutes down,, under 40 ℃, reacted 60 minutes then, make crystal seed with salt acid for adjusting pH value to 4 at 50 ℃.
(2) preparation of rutile titanium dioxide
With 1000 kilograms of anatase titanium dioxides (eastern good BA01-01 that Dong Jia company in Shandong produces, the scope of particle dia is 300-400nm) and 100 gram crystal seeds (with dry weight basis), 8 gram Quilonum Retards, 6 gram magnesium oxide mix, and the mixture that mixing is obtained is in muffle furnace, 200 ℃ of heating 10 minutes down, is warmed up to 800 ℃ of insulations 3 hours then, cooling obtains product A 4.
Measure scope, crystal formation and the particle diameter of the particle dia of product A 4 according to the method for embodiment 1.The result is as shown in table 1.
Embodiment 5
Present embodiment illustrates the preparation method of rutile titanium dioxide of the present invention.
(1) preparation of crystal seed
The metatitanic acid, 2400 of 1000 grams is restrained water and 50 gram zinc oxide mixing stirrings, reacted 40 minutes down,, under 40 ℃, reacted 60 minutes then, make crystal seed with salt acid for adjusting pH value to 4 at 50 ℃.
(2) preparation of rutile titanium dioxide
With 1000 kilograms of anatase titanium dioxides (eastern good BA01-01 that Dong Jia company in Shandong produces, the scope of particle dia is 300-400nm) and 100 gram crystal seeds (with dry weight basis), 10 gram Lithium Sulphates, 9 gram lime carbonate, 8 gram magnesium oxide, 2 gram tindioxide mix, and the mixture that mixing is obtained is in muffle furnace, 200 ℃ of heating 10 minutes down, is warmed up to 800 ℃ of insulations 2.5 hours then, cooling obtains product A 5.
Measure scope, crystal formation and the particle diameter of the particle dia of product A 5 according to the method for embodiment 1.The result is as shown in table 1.
Embodiment 6
Present embodiment illustrates the preparation method of rutile titanium dioxide of the present invention.
(1) preparation of crystal seed
The metatitanic acid, 2400 of 1000 grams is restrained water and 50 gram zinc oxide mixing stirrings, reacted 40 minutes down,, under 40 ℃, reacted 60 minutes then, make crystal seed with salt acid for adjusting pH value to 4 at 50 ℃.
(2) preparation of rutile titanium dioxide
With 1000 kilograms of anatase titanium dioxides (eastern good BA01-01 that Dong Jia company in Shandong produces, the scope of particle dia is 300-400nm) and 100 gram crystal seeds (with dry weight basis), 5 gram Lithium Sulphates mix, and the mixture that mixing is obtained is in muffle furnace, heated 10 minutes down at 200 ℃, be warmed up to 800 ℃ of insulations 2 hours then, cooling obtains product A 5.
Measure scope, crystal formation and the particle diameter of the particle dia of product A 6 according to the method for embodiment 1.The result is as shown in table 1.
Embodiment 7
Method according to embodiment 1 prepares rutile titanium dioxide, and different is, during the preparation of crystal seed: adopt 30 gram zinc carbonates to substitute zinc oxide.Finally obtain product A 7.Measure scope, crystal formation and the particle diameter of the particle dia of product A 7 according to the method for embodiment 1.The result is as shown in table 1.
Embodiment 8
Method according to embodiment 1 prepares rutile titanium dioxide, and different is, during the preparation of rutile titanium dioxide: Quilonum Retard 10.2 grams, magnesium oxide 10.5 grams, zinc oxide 9 grams, 0.3 gram tindioxide.Finally obtain product A 8.Measure scope, crystal formation and the particle diameter of the particle dia of product A 8 according to the method for embodiment 1.The result is as shown in table 1.
Embodiment 9
Method according to embodiment 1 prepares rutile titanium dioxide, and different is, during the preparation of crystal seed: the consumption of water is 2800 grams.Finally obtain product A 9.Measure scope, crystal formation and the particle diameter of the particle dia of product A 9 according to the method for embodiment 1.The result is as shown in table 1.
Embodiment 10
Method according to embodiment 1 prepares rutile titanium dioxide, and different is that the preparation method of described crystal seed is: the metatitanic acid, 1800 of 1000 grams is restrained water and 55 gram zinc oxide mixing stirrings, reacted 140 minutes down at 70 ℃, make crystal seed.Finally obtain product A 10.Measure scope, crystal formation and the particle diameter of the particle dia of product A 10 according to the method for embodiment 1.The result is as shown in table 1.
Comparative Examples
Method according to embodiment 1 prepares rutile titanium dioxide, different is, during rutile titanium dioxide: with 1000 kilograms of anatase titanium dioxides (eastern good BA01-01 that Dong Jia company in Shandong produces, the scope of particle dia is 300-400nm) and 150 gram crystal seeds (with dry weight basis), 6 gram lime carbonate, 8 gram magnesium oxide, 10.5 the gram tindioxide mixes, and the mixture that mixing is obtained is in muffle furnace, heated 10 minutes down at 200 ℃, be warmed up to 900 ℃ of insulations 3.5 hours then, cooling obtains product D.
Measure scope, crystal formation and the particle diameter of the particle dia of product D according to the method for embodiment 1.The result is as shown in table 1.
Table 1
Numbering | The scope of particle dia (nm) | Transformation efficiency (%) |
??A1 | ??300-450 | ??100.00 |
??A2 | ??300-450 | ??99.32 |
??A3 | ??300-500 | ??98.23 |
??A4 | ??300-450 | ??98.58 |
??A5 | ??300-500 | ??98.63 |
??A6 | ??300-550 | ??98.07 |
??A7 | ??300-450 | ??98.51 |
??A8 | ??300-450 | ??99.10 |
??A9 | ??300-500 | ??99.04 |
??A10 | ??300-450 | ??99.35 |
??D | ??300-700 | ??90.26 |
As can be seen from Table 1, the transformation efficiency of the rutile titanium dioxide of method of the present invention is very high, can arrive more than 98%.In addition, because selected crystal type promoting reagent impels titanium dioxide by the fast transition of anatase titanium dioxide to rutile-type, thereby make the high-temperature calcination time shorter, and because the carbon dioxide that carbonate is discharged in reaction, thereby the particle diameter of the rutile titanium dioxide that method of the present invention makes and the particle diameter of raw material anatase titanium dioxide are more or less the same, in addition, the rutile titanium dioxide of gained is comparatively loose, and is easy to use.
Claims (13)
1. a rutile titanium dioxide is characterized in that, contains zn cpds and lithium compound in the described rutile titanium dioxide.
2. rutile titanium dioxide according to claim 1 is characterized in that, in the described rutile titanium dioxide, with Li
+Meter, the content of described lithium compound accounts for the 0.1-1 quality % of rutile titanium dioxide; With Zn
2+Meter, the content of described zn cpds accounts for the 0.1-0.8 quality % of rutile titanium dioxide.
3. rutile titanium dioxide according to claim 1 is characterized in that, also contains at least a in magnesium compound, the tin compound in the described rutile titanium dioxide.
4. rutile titanium dioxide according to claim 3, it is characterized in that, in the described rutile titanium dioxide, the content of magnesium compound accounts for the 0.1-1.2 quality % of rutile titanium dioxide, and the content of tin compound accounts for the 0.03-0.2 quality % of rutile titanium dioxide.
5. the preparation method of a rutile titanium dioxide is characterized in that, this method comprises that the mixture roasting that will contain anatase titanium dioxide, rutile titanium dioxide crystal seed and lithium salts obtains rutile titanium dioxide; The described method for preparing the rutile titanium dioxide crystal seed comprises: in the presence of water, metatitanic acid is contacted with zinc salt, the temperature of contact is 40-80 ℃.
6. method according to claim 5 is characterized in that, the method for preparing the rutile titanium dioxide crystal seed comprises: the metatitanic acid with 100 weight parts is a benchmark, and the consumption of described zinc salt is the 1-10 weight part, and the consumption of water is the 100-250 weight part.
7. method according to claim 5 is characterized in that, the method for preparing the rutile titanium dioxide crystal seed comprises: described zinc salt is one or more in zinc oxide, zinc carbonate, zinc chloride, zinc sulfate, the zinc nitrate.
8. method according to claim 5 wherein, is a benchmark with the anatase titanium dioxide of 100 weight parts, and with dry weight basis, the consumption of described rutile titanium dioxide crystal seed is the 5-15 weight part, and the consumption of lithium salts is the 0.3-3 weight part.
9. method according to claim 5 is characterized in that, also contains carbonate in the described mixture.
10. method according to claim 9 is characterized in that, is benchmark with the anatase titanium dioxide of 100 weight parts, and with dry weight basis, the consumption of described carbonate is the 0.5-4 weight part.
11. method according to claim 5 is characterized in that, also contains in magnesium oxide, zinc oxide, the tindioxide one or more in the described mixture.
12. method according to claim 11, it is characterized in that, anatase titanium dioxide with 100 weight parts is a benchmark, with dry weight basis, described magnesian consumption is the 0.2-3 weight part, the consumption of described zinc oxide is the 0.2-2.5 weight part, and the consumption of described tindioxide is the 0.02-0.2 weight part.
13. method according to claim 5 is characterized in that, the temperature of described roasting is 700-900 ℃, and the time of roasting is 1-5 hour.
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CN103429536A (en) * | 2011-04-28 | 2013-12-04 | 石原产业株式会社 | Method for producing lithium titanate precursor, method for producing lithium titanate, lithium titanate, electrode active substance, and storage device |
CN104591274A (en) * | 2015-01-09 | 2015-05-06 | 攀钢集团攀枝花钢铁研究院有限公司 | Calcining method for preparing rutile-type titanium dioxide powder |
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CN106241862B (en) * | 2016-08-22 | 2018-03-23 | 东南大学 | A kind of method for preparing single dispersing rutile type nano titanic oxide |
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CN109928425B (en) * | 2019-04-23 | 2021-09-17 | 广西民族大学 | Method for reducing calcination temperature of metatitanic acid converted into rutile type titanium dioxide |
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