CN100368302C - Rutile-type titanium white and its prepn process - Google Patents
Rutile-type titanium white and its prepn process Download PDFInfo
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- CN100368302C CN100368302C CNB2006100203340A CN200610020334A CN100368302C CN 100368302 C CN100368302 C CN 100368302C CN B2006100203340 A CNB2006100203340 A CN B2006100203340A CN 200610020334 A CN200610020334 A CN 200610020334A CN 100368302 C CN100368302 C CN 100368302C
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Abstract
The present invention provides a rutile type titanium pigment and a preparing method thereof, which belongs to the filed of chemical industry. The quantity of rutile type TiO2 in the rutile type titanium pigment is not less than 99%, and the quantity of a blue phase in the rutile type titanium pigment is not less than 2.5; quality indexes, such as reducing power, brightness value, etc., of the rutile type titanium pigment are high. The preparing technology of the rutile type titanium pigment comprises the steps that 0.20% to 0.70% of zirconium ion solution is added before a combined salt treatment agent is added into metatitanic acid slurry; the addition quantity of the zirconium ion solution is the weight percentage of ZrO2 in the total quantity of TiO2. Based on the existing method, the preparing method of the present invention is creatively improved and has the advantages of simple step, sufficient utilization of the existing equipment, etc.; the titanium pigment with quality obviously increased can be obtained, and a big problem in the filed is solved. The preparing method can be used in the production line of titanium pigment with a sulfuric acid method to generate high-grade rutile type pigment titanium white, and has an extremely good application prospect.
Description
Technical field
The invention belongs to chemical field, be specifically related to a kind of Rutile type Titanium Dioxide and preparation method thereof.
Background technology
Rutile type Titanium Dioxide with Production By Sulfuric Acid Process, be a certain amount of salt treatment agent to be added contain in the metatitanic acid of rutile type calcining seeds, carry out high-temperature calcination after mixing, generate the titanium dioxide with rutile crystal type structure Ti O2, further processing treatment is with the preparation related products.
In " sulfuric acid process is produced the novel process research of Rutile type Titanium Dioxide " (" chemical industry mineral and processing " the 8th phase in 1999) literary composition, disclose and be used phosphorus compound and potassium compound prepares titanium dioxide for the salt treatment agent; It is the titanium dioxide of the technology preparation of ZnO, MgO that Chinese patent ZL91108973.X " the introducing iron protochloride prepares rutile titanium dioxide " discloses crystal type promoting reagent; In Chinese patent 200410021800.8 " a kind of preparation method of Rutile type Titanium Dioxide ", disclose by potassium compound, phosphorus compound, aluminum compound be the crystal formation control agent technology with the preparation titanium dioxide; Disclose with ZnSO in (" Hebei chemical industry " third phase nineteen ninety) " add combination promotor and prepare Rutile type Titanium Dioxide "
4, K
2CO
3, H
3PO
4For combination salt treatment agent prepares titanium dioxide.
All there is rutile TiO in existing disclosed titanium dioxide
2Content, reducing power (Tcs) and the blue phase inharmonic shortcomings of quality index such as (Scx), that is: 1, when rutile content increases and greater than 99% the time, blue phase (Scx) and reducing power (Tcs) be decline obviously, causes the reducing power value less than 1750, indigo plant is worth mutually less than 2.0; 2, in the time of will increasing mutually blue and reducing power (Tcs) value, TiO
2Rutile content can corresponding reduction.In addition, existing salt processing method makes the high-temperature calcination poor-performing of metatitanic acid, and metatitanic acid easily produces burning or underburnt, and the titanium dioxide primary product reducing power value that both of these case all can cause making is less than 1750, and indigo plant is worth mutually also less than 2.0.Therefore, provide a kind of rutile TiO
2The titanium dioxide that content, reducing power and blue equal mass index all can remain on higher level is the active demand of this area.
Summary of the invention
First purpose of the present invention provides a kind of titanium dioxide.The rutile TiO of this titanium dioxide
2Content is not less than 99%, and it is 2.5～4.0 that indigo plant is worth (Scx) mutually.
Further, the reducing power value (Tcs) of this titanium dioxide is 1770～1930.
Second purpose of the present invention provides a kind of method for preparing above-mentioned titanium dioxide.This method is to add to add 0.20%～0.70% zirconium ion solution before the combination salt treatment agent earlier in the metatitanic acid slurry, and wherein the add-on of zirconium ion solution is meant with ZrO
2Meter accounts for TiO in the metatitanic acid
2The weight percent of total amount.
Further, this method may further comprise the steps:
A, with the zirconium ion solution that adds 0.20%～0.70% in the metatitanic acid slurry, mix, wherein the add-on of zirconium ion solution is meant with ZrO
2Meter accounts for TiO in the metatitanic acid
2The weight percent of total amount;
B, adding zine ion solution or oxide powder and zinc slurry behind phosphoric acid solution and the potassium ion solution, mix;
C, be to calcine 90min～210min under 830 ℃～920 ℃ the condition in temperature, promptly get the Rutile type Titanium Dioxide first product;
Wherein, described metatitanic acid is the metatitanic acid that contains rutile type calcining seeds.
Further, above-mentioned zirconium ion solution is zirconium sulfate solution or zirconium oxychloride solution.
The add-on of the zine ion solution described in the aforesaid method step b is 0.20%～0.90%; Wherein the add-on of zine ion solution is meant in ZnO and accounts for TiO in the metatitanic acid
2Weight percent.
Further, above-mentioned zine ion solution is liquor zinci chloridi.
The add-on of phosphoric acid solution is 0.05%～0.15% among the step b of aforesaid method, and wherein the add-on of phosphoric acid solution is meant with P
2O
5Meter accounts for TiO in the metatitanic acid
2Weight percent.
The add-on of potassium ion solution is 0.20%～0.70% among the aforesaid method step b, and wherein the add-on of potassium ion solution is meant with K
2The O meter accounts for TiO in the metatitanic acid
2Weight percent.
Further, above-mentioned potassium ion solution is K
2CO
3Solution or KOH solution.
Specifically, the inventive method can be implemented by following step: take by weighing metatitanic acid and put into container, add deionized water and be diluted to TiO under agitation condition
2300～380g/L (the too low increase calcinating consumption of concentration, too high be difficult for stirring) adds weight percent for containing the rutile type calcining seeds metatitanic acid (with TiO
2Meter) 0.20%～0.70% zirconium sulfate solution or zirconium oxychloride solution are (with ZrO
2Meter), stir.Add weight percent then for containing the rutile type calcining seeds metatitanic acid (with TiO
2Meter) 0.20%～0.90% oxide powder and zinc slurry or liquor zinci chloridi (in ZnO) add weight percent for containing the rutile type calcining seeds metatitanic acid (with TiO
2Meter) 0.05%～0.15% phosphoric acid solution is (with P
2O
5Meter), weight percent is for containing the rutile type calcining seeds metatitanic acid (with TiO
2Meter) 0.20%～0.70% K
2CO
3Solution or KOH solution are (with K
2The O meter).Add immediately after stirring in the baking oven, dry under 120 ℃～160 ℃, again with this areas such as resistance furnace calciner commonly used, at 830 ℃～920 ℃ calcining 90min～210min, promptly.
Titanium dioxide provided by the invention has overcome the rutile TiO that existing Rutile type Titanium Dioxide exists
2Content, reducing power (Tcs) and the blue phase inharmonic shortcomings of index such as (Scx); Its rutile TiO
2Amount is not less than 99%, and reducing power is not less than 1770, and indigo plant is not less than 2.5 mutually, and brightness value is not less than 94.5, and loose pure white easy pulverizing has better quality, can be widely used in producing high-grade rutile titanium white powder and related products.The method for preparing titanium dioxide provided by the invention, be before present salt processing method, to have added zirconium ion solution earlier to handle, have step simple, can make full use of advantage such as existing installation, can obtain the titanium dioxide that quality obviously improves, solved a great problem of this area, can be used on the sulfuric acid method titanium pigment production line having fabulous application prospect to produce high-grade rutile pigment titanium white.
Obviously, according to foregoing of the present invention,,, can also make modification, replacement or the change of other various ways not breaking away under the above-mentioned basic fundamental thought of the present invention prerequisite according to the ordinary skill knowledge and the customary means of this area.
By following embodiment foregoing of the present invention further being described in detail, is limiting the scope of the invention but should not be construed as.
Embodiment
The preparation of embodiment 1 titanium dioxide of the present invention
Take by weighing the 278g metatitanic acid (with TiO
2Meter 100g) puts into beaker, under agitation condition, add deionized water and be diluted to TiO
2340g/L.
Then, add weight percent for containing the rutile type calcining seeds metatitanic acid (with TiO
2Meter) 0.20% zirconium sulfate solution is (with ZrO
2Meter), add weight percent again for containing the rutile type calcining seeds metatitanic acid (with TiO
2Meter) 0.20% ZnO powder slurry (in ZnO), weight percent is for containing the rutile type calcining seeds metatitanic acid (with TiO
2Meter) 0.05% phosphoric acid solution is (with P
2O
5Meter), weight percent is for containing the rutile type calcining seeds metatitanic acid (with TiO
2Meter) 0.20% solution of potassium carbonate is (with K
2The O meter).
The aforesaid liquid stirring after 60 minutes, is added in the baking oven immediately, and drying is put into resistance furnace more than 4 hours again under 120 ℃～140 ℃, calcines 3.5 hours, and makes titanium dioxide A for 830 ℃.
The preparation of embodiment 2 titanium dioxides of the present invention
Take by weighing the 278g metatitanic acid (with TiO
2Meter 100g) puts into beaker, under agitation condition, add deionized water and be diluted to TiO
2350g/L.
Then, add weight percent for containing the rutile type calcining seeds metatitanic acid (with TiO
2Meter) 0.35% zirconium sulfate solution is (with ZrO
2Meter), add weight percent again for containing the rutile type calcining seeds metatitanic acid (with TiO
2Meter) 0.45% ZnO powder slurry (in ZnO), weight percent is for containing the rutile type calcining seeds metatitanic acid (with TiO
2Meter) 0.10% phosphoric acid solution is (with P
2O
5Meter), weight percent is for containing the rutile type calcining seeds metatitanic acid (with TiO
2Meter) 0.35% solution of potassium carbonate is (with K
2The O meter).
Above-mentioned gained liquid agitation after 50 minutes, is added in the baking oven immediately, and drying is put into resistance furnace more than 4 hours again under 120 ℃～140 ℃, calcines 2.5 hours, and makes titanium dioxide B for 870 ℃.
The preparation of embodiment 3 titanium dioxides of the present invention
Take by weighing the 278g metatitanic acid (with TiO
2Meter 100g) pours in the beaker, under agitation condition, add deionized water and be diluted to TiO
2380g/L.
Then, add weight percent for containing the rutile type calcining seeds metatitanic acid (with TiO
2Meter) 0.70% zirconium sulfate solution is (with ZrO
2Meter), add weight percent again for containing the rutile type calcining seeds metatitanic acid (with TiO
2Meter) 0.90% ZnO powder slurry (in ZnO), weight percent is for containing the rutile type calcining seeds metatitanic acid (with TiO
2Meter) 0.15% phosphoric acid solution is (with P
2O
5Meter), weight percent is for containing the rutile type calcining seeds metatitanic acid (with TiO
2Meter) 0.70% solution of potassium carbonate is (with K
2The O meter).
Above-mentioned gained liquid agitation after 40 minutes, is added in the baking oven immediately, and drying is put into resistance furnace more than 3.5 hours again under 140 ℃～160 ℃, calcines 1.5 hours, and makes titanium dioxide C for 920 ℃.
The preparation of embodiment 4 titanium dioxides of the present invention
Take by weighing the 278g metatitanic acid (with TiO
2Meter 100g) pours in the beaker, under agitation condition, add deionized water and be diluted to TiO
2340g/L.
Then, add weight percent for containing the rutile type calcining seeds metatitanic acid (with TiO
2Meter) 0.40% zirconium sulfate solution is (with ZrO
2Meter), add weight percent again for containing the rutile type calcining seeds metatitanic acid (with TiO
2Meter) 0.45% ZnO powder slurry (in ZnO), weight percent is for containing the rutile type calcining seeds metatitanic acid (with TiO
2Meter) 0.10% phosphoric acid solution is (with P
2O
5Meter), weight percent is for containing the rutile type calcining seeds metatitanic acid (with TiO
2Meter) 0.40% solution of potassium carbonate is (with K
2The O meter).
Above-mentioned gained liquid agitation after 40 minutes, is added in the baking oven immediately, and drying is put into resistance furnace more than 4 hours again under 140 ℃～160 ℃, calcines 2.0 hours, and makes titanium dioxide D for 860 ℃.
The preparation of embodiment 5 titanium dioxides of the present invention
Take by weighing the 278g metatitanic acid (with TiO
2Meter 100g) pours in the beaker, under agitation condition, add deionized water and be diluted to TiO
2330g/L.
Then, add weight percent for containing the rutile type calcining seeds metatitanic acid (with TiO
2Meter) 0.35% zirconium oxychloride solution is (with ZrO
2Meter), add weight percent again for containing the rutile type calcining seeds metatitanic acid (with TiO
2Meter) 0.40% liquor zinci chloridi (in ZnO), weight percent is for containing the rutile type calcining seeds metatitanic acid (with TiO
2Meter) 0.10% phosphoric acid solution is (with P
2O
5Meter), weight percent is for containing the rutile type calcining seeds metatitanic acid (with TiO
2Meter) 0.35% potassium hydroxide solution is (with K
2The O meter).
Above-mentioned gained liquid agitation after 40 minutes, is added in the baking oven immediately, and drying is put into resistance furnace more than 4 hours again under 130 ℃～150 ℃, calcines 2.5 hours for 860 ℃.Hour, make titanium dioxide E.
The preparation of embodiment 6 titanium dioxides of the present invention
Take by weighing the 278g metatitanic acid (with TiO
2Meter 100g) pours in the beaker, under agitation condition, add deionized water and be diluted to TiO
2360g/L.
Then, add weight percent for containing the rutile type calcining seeds metatitanic acid (with TiO
2Meter) 0.60% zirconium sulfate solution is (with ZrO
2Meter), add weight percent again for containing the rutile type calcining seeds metatitanic acid (with TiO
2Meter) 0.45% liquor zinci chloridi (in ZnO), weight percent is for containing the rutile type calcining seeds metatitanic acid (with TiO
2Meter) 0.10% phosphoric acid solution is (with P
2O
5Meter), weight percent is for containing the rutile type calcining seeds metatitanic acid (with TiO
2Meter) 0.40% potassium hydroxide solution is (with K
2The O meter).
Above-mentioned gained liquid agitation after 40 minutes, is added in the baking oven immediately, and drying is put into resistance furnace more than 4 hours again under 130 ℃～150 ℃, calcines 2 hours, and makes titanium dioxide F for 880 ℃.
The quality examination of test example 1 titanium dioxide of the present invention
1, detecting instrument and method:
Rutile TiO
2Content D/max-RC type x-ray diffractometer (Japanese Rigaku Denki Co., Ltd) detection computations.
Detect each sample tristimulus values x by the differential chromascope
1, y
1, z
1, again according to the measured value x of standard specimen (R902 of Du Pont)
0, y
0, z
0Be worth (Scx), reducing power (Tcs), brightness value (Jasn%) mutually with the set-point of this standard specimen and the indigo plant that calculates each testing sample.
Method of calculation following (subscript of formula: " giving " is the set-point of standard specimen, and " mark " is the standard specimen value, and " sample " is sample value):
Reducing power (Tcs): Tcs
Sample=Tcs
Give-(y
0-y
1) * 100
Brightness value (Jasn%): brightness value
Sample=y
1+ y '
Wherein: modified value y '=Jasn%
Give-y
0
Indigo plant is worth (Scx): Scx mutually
Sample=(z
1-x
1)-Scx
Mark
Scx
Mark=(z
0-x
0)-Scx
Give
2, the sample of Jian Ceing:
Titanium dioxide A, B, C, D, E that the foregoing description 1～6 is prepared;
Commercially available rutile TiO
2Product F;
Identical with other steps with the embodiment of the invention 6 methods, only do not add the prepared titanium dioxide G of method of zirconium ion solution.
3, detected result:
Detect the rutile TiO of above-mentioned A, B, C, D, E, F, G titanium dioxide respectively
2Indexs such as content, indigo plant are worth mutually, reducing power value, brightness value, detected result sees Table 1:
Table 1: titanium dioxide primary product quality examination result
| Rutile TiO 2Content | Indigo plant is worth (Scx) mutually | Reducing power value (Tcs) | Brightness value (Jasn%) | |
| A | ＞99％ | 2.5 | 1820 | 94.5 |
| B | ＞99％ | 2.9 | 1880 | 94.8 |
| C | ＞99％ | 2.6 | 1840 | 94.6 |
| D | ＞99％ | 2.8 | 1870 | 94.7 |
| E | ＞99％ | 2.7 | 1860 | 94.6 |
| F | ＞99％ | 2.0 | 1770 | 94.3 |
| G | 96.5％ | 1.6 | 1680 | 93.8 |
(by this area convention, when the rutile TiO that records
2The value of content is higher than at 99% o'clock, represents rutile TiO in examining report with rutile content＞99%
2Content is lower than at 99% o'clock and then uses concrete numeral.)
By above-mentioned example as seen, Rutile type Titanium Dioxide of the present invention has overcome the rutile TiO that existing Rutile type Titanium Dioxide exists
2Content, reducing power (Tcs) and the blue phase inharmonic shortcomings of quality index such as (Scx).Rutile TiO wherein
2Content is not less than 99%; Reducing power is not less than 1770, reaches as high as 1930; Indigo plant is not less than 2.5 mutually, reaches as high as 4.0; Brightness value also is not less than 94.5, the outward appearance pure white easy pulverizing of loosening, and its overall quality index is better than currently available products greatly.The present invention prepares the method for titanium dioxide and is creatively improved on the basis of existing method, have step simple, with low cost, can make full use of advantages such as existing installation, can be used on the sulfuric acid method titanium pigment production line having fabulous application prospect to produce high-grade rutile pigment titanium white.
Claims (8)
1. method for preparing Rutile type Titanium Dioxide is characterized in that: add in the metatitanic acid slurry and add 0.20%～0.70% zirconium ion solution before the combination salt treatment agent earlier, wherein the add-on of zirconium ion solution is meant with ZrO
2Meter accounts for TiO in the metatitanic acid
2The weight percent of total amount.
2. the method for preparing titanium dioxide according to claim 1 may further comprise the steps:
A, with the zirconium ion solution that adds 0.20%～0.70% in the metatitanic acid slurry, mix, wherein the add-on of zirconium ion solution is meant with ZrO
2Meter accounts for TiO in the metatitanic acid
2The weight percent of total amount;
B, adding zine ion solution or oxide powder and zinc slurry behind phosphoric acid solution and the potassium ion solution, mix;
C, be to calcine 90min～210min under 830 ℃～920 ℃ the condition in temperature, promptly;
Wherein, described metatitanic acid is the metatitanic acid that contains rutile type calcining seeds.
3. method according to claim 2 is characterized in that: the zirconium ion solution described in the step a is zirconium sulfate solution or zirconium oxychloride solution.
4. method according to claim 2 is characterized in that: the add-on of the zine ion solution described in the step b is 0.20%～0.90%; Wherein the add-on of zine ion solution is meant in ZnO and accounts for TiO in the metatitanic acid
2Weight percent.
5. method according to claim 4 is characterized in that: described zine ion solution is liquor zinci chloridi.
6. method according to claim 2 is characterized in that: the add-on of phosphoric acid solution is 0.05%～0.15% among the step b, and wherein the add-on of phosphoric acid solution is meant with P
2O
5Meter accounts for TiO in the metatitanic acid
2Weight percent.
7. method according to claim 2 is characterized in that: the add-on of potassium ion solution is 0.20%～0.70% among the step b, and wherein the add-on of potassium ion solution is meant with K
2The O meter accounts for TiO in the metatitanic acid
2Weight percent.
8. method according to claim 7 is characterized in that: described potassium ion solution is K
2CO
3Solution or KOH solution.
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| CN101463195B (en) * | 2007-12-21 | 2011-09-21 | 衡阳天友化工有限公司 | Red schorl type titanium dioxide coating method and preparation of used reagent |
| CN101613124B (en) * | 2008-06-26 | 2011-11-16 | 比亚迪股份有限公司 | Method for preparing rutile titanium dioxide |
| CN102745740B (en) * | 2012-07-18 | 2014-02-05 | 云南昆欧科技有限责任公司 | Titanium dioxide treating agent |
| CN104817105B (en) * | 2015-04-21 | 2017-01-11 | 江苏镇钛化工有限公司 | Preparation method for treating titanium white by high zinc salt |
| CN104891564A (en) * | 2015-05-04 | 2015-09-09 | 四川龙蟒钛业股份有限公司 | Preparation method of high-whiteness high-brightness raw rutile titanium dioxide |
| CN108408770B (en) * | 2018-06-08 | 2020-05-22 | 龙蟒佰利联集团股份有限公司 | Sulfur removal production process for metatitanic acid |
| CN108929574A (en) * | 2018-09-08 | 2018-12-04 | 江苏中研创星材料科技有限公司 | A kind of preparation method of the dedicated high-grade titanium dioxide of papermaking |
| CN110564181A (en) * | 2019-08-26 | 2019-12-13 | 中东金润新材料有限公司 | production process of composite high-coating titanium dioxide |
| CN111252808A (en) * | 2020-03-31 | 2020-06-09 | 广西金茂钛业有限公司 | Method for preparing special rutile titanium dioxide for high-weather-resistance plastics |
| CN111849269A (en) * | 2020-07-28 | 2020-10-30 | 东来涂料技术（上海）股份有限公司 | Water-based high-covering high-weather-resistance white finish paint for automobiles and preparation method thereof |
| CN112175420A (en) * | 2020-10-09 | 2021-01-05 | 安徽金星钛白（集团）有限公司 | Rutile type titanium dioxide crude product with high light resistance and preparation method and application thereof |
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