CN104843782A - Preparation method of high-whiteness light-resistance rutile type titanium dioxide substrate - Google Patents
Preparation method of high-whiteness light-resistance rutile type titanium dioxide substrate Download PDFInfo
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Abstract
The invention discloses a preparation method of high-whiteness light-resistance rutile type titanium dioxide substrate. The preparation method includes steps of primary washing of metatitanic acid, preparation of metatitanic acid sizing, bleaching of metatitanic acid sizing, secondary washing of metatitanic acid, salt treating, roasting and smashing. In the bleaching of metatitanic acid sizing, 5wt% of rutile titanium dioxide roasted seed crystal and 0.2wt% of Ti3 and solution are added into the sizing. In the step of salt treating, potassium compound, phosphorous compound, aluminum compound and stibium oxide are added into the secondarily-washed metatitanic acid. By adding aluminum salt content, aluminum salt enters crystal lattice during growth of titanium dioxide crystal, light resistance performance of titanium dioxide pigment is substantially improved, and the yellowish problem caused by increment of aluminum slat content can be eliminated by adding antimonic salt, so that whiteness of dry powder is kept, whiteness and light resistance are kept balanced, and the high-whiteness light-resistance rutile type titanium dioxide substrate.
Description
Technical field
The present invention relates to a kind of preparation method of high whiteness light-fastness rutile type silicon dioxide substrate, belong to titanium white powder pigment applied technical field.
Background technology
Titanium dioxide, is commonly called as titanium dioxide, has the advantages such as the physicochemical property of high whiteness, opacity and excellence, is widely used in the fields such as plastics, coating, ink and papermaking.Pigment art is as one of the main application fields of titanium dioxide, and wherein decorative paper production field has higher requirement to the photostabilization of titanium dioxide and whiteness.
Decorative paper production application hot press forming technology, in preparation process by by titanium dioxide together with fiber through thermosetting resin dipping, then hot-formingly obtain finished product.By the laminated paper of this technique gained, there is impact resistance, the feature such as heat-resisting and fine and close, but for titanium dioxide, this laminated paper compact structure, when being subject to extraneous ultraviolet irradiation, the titanic on its surface is easily reduced to titanous, causes goods easily to gray.Therefore in order to titanium dioxide being applied to field of papermaking, in titanium white production, improve titanium dioxide anti-tarnishing ability and photostabilization seem very important.
The Traditional Industrialization production method of titanium dioxide is generally divided into sulfuric acid process and chlorination process, wherein the main raw material of Titanium White Production By Sulfuric Acid Process is ilmenite and sulfuric acid, and main technological steps is: ilmenite and sulfuric acid solution obtain titanyl sulfate, generate metatitanic acid through sedimentation, crystallization, hydrolysis; Metatitanic acid through one washing, bleaching, two to wash, Ficus caricaL, calcination obtain rutile titanium dioxide base material; Silicon dioxide substrate, through wet-milling, sand milling, the gentle powder of coating, obtains titanium dioxide product.
In the prior art, in order to improve whiteness and the photostabilization of titanium dioxide product, generally that envelope membrane surface process is carried out to silicon dioxide substrate, join in the slurry of titanium dioxide as US Patent No. 2004025749 discloses with the compound of phosphoric acid salt, titanium and aluminium, improve the anti-tarnishing ability of titanium dioxide, in paper and laminated paper field, there is good effect; And for example US Patent No. 5785748 adopts aluminum compound and phosphoric acid to be mixed with mixing solutions in a heated condition, join in Titanium dioxide slurry after dilution, then pH value is adjusted to 3-3.5, thus make treatment agent be deposited in titanium dioxide surface, additional Potassium Iodate, potassium sulfate or the saltpetre of adding, in raw material, can make the photostabilization of pigment be improved again simultaneously.The shortcoming of this method is, needs to add a large amount of phosphoric acid in system, and not only cause the wasting of resources, too increase the production cost of titanium dioxide, commercial value is limited.
For another example Chinese invention patent CN101857736A and CN102585559A discloses to adopt and in titania slurry, adds the compounds such as zirconium compounds, silicon compound and aluminium to improve the light fastness of titanium dioxide, these patents are all improved whiteness and the photostabilization of titanium dioxide by coating means, but adopt multiple compounds coating inherently can not increase substantially photostabilization, we inherently should improve in the photostabilization of silicon dioxide substrate and whiteness and set about considering.
Summary of the invention
Object of the present invention is just for above-mentioned the deficiencies in the prior art, provides the preparation method of a kind of high whiteness and sunproof rutile titanium dioxide base material.
To achieve these goals, the technical solution used in the present invention is such:
A preparation method for high whiteness light-fastness rutile type silicon dioxide substrate, comprises the following steps:
(1) metatitanic acid is prepared: ilmenite and sulfuric acid solution obtain titanyl sulfate, generate metatitanic acid through sedimentation, crystallization, hydrolysis;
(2) metatitanic acid is once washed: the deionized water wash metatitanic acid by temperature being 50 ~ 80 DEG C, removes metallic impurity wherein;
(3) prepare metatitanic acid slurry: add water in the metatitanic acid after washing making beating, the concentration of slurry is 300 ~ 350g/L;
(4) bleach metatitanic acid slurry: in metatitanic acid slurry, add sulfuric acid, make the sulfuric acid concentration of slurry be 60 ~ 90g/L, and in slurry, add the rutile type calcining seeds of 5wt% and the Ti of 0.2wt% simultaneously
3+solution, weight percent metering benchmark is the total mass of titanium dioxide in metatitanic acid slurry, described Ti
3+the concentration of solution is 0.6g/L;
(5) metatitanic acid secondary washing: by the metatitanic acid slurry of reduction bleaching, filter with the leaf filter of negative pressure of vacuum or rotary vacuum drum filter midge, be the deionized water wash metatitanic acid of 50 ~ 80 DEG C again by temperature, wash away ferrous sulfate further, to reduce the content of iron, until the content of metatitanic acid ferrous ions is less than 20ppm;
(6) Ficus caricaL: add water the metatitanic acid after secondary washing making beating, and the concentration of slurry is 300 ~ 350g/L; The sb oxide of the potassium compound of 0.27wt%, the phosphorus compound of 0.2wt%, the aluminum compound of 0.4-0.8wt% and 0.15wt% is once added in metatitanic acid slurry, mix, its weight percent metering benchmark is two total masses of washing titanium dioxide in metatitanic acid slurry, and potassium compound add-on is with K
2o counts, and phosphorus compound add-on is with P
2o
5meter, aluminum compound add-on is with Al
2o
3meter, sb oxide add-on is with Sb
2o
3meter;
(6) calcining is pulverized: above-mentioned metatitanic acid de-watering of slurries calcining, calcining temperature controls between 1050 DEG C ~ 1080 DEG C, and after calcining, namely pulverizing obtains rutile titanium dioxide base material.
Described potassium compound is selected from potassium hydroxide, salt of wormwood and saltpetre.
Described phosphorus compound is selected from phosphoric acid, Sodium hexametaphosphate 99 and ammonium phosphate.
Described aluminum compound is selected from Tai-Ace S 150, aluminum chloride and sodium metaaluminate.
Described sb oxide is antimonous oxide.
As everyone knows, metatitanic acid needs at high temperature long-time calcining just can change rutile-type crystal formation into, this will cause particle aggregation or sintering, cause product lattice imperfection too much, crystal grain is excessive and very hard, and then affect the dispersiveness of product, opacifying power and pigment performance, high-temperature operation simultaneously also brings certain difficulty to Producing Titanium Dioxide, thus, obtain the Rutile type Titanium Dioxide of excellent property, the processing condition that metatitanic acid of must controlling well in process of production transforms, rutile type calcining seeds adds in the metatitanic acid before calcining by the present invention, when calcination processing, Induction Transformation is played in the process that this crystal seed is transformed to rutile-type by anatase titanium dioxide at titanium dioxide, thus reduce invert point, make pigment particles profile round and smooth simultaneously, pigment performance is superior.
Metatitanic acid adds the process that a small amount of chemical additives of people carries out modification before calcination, is called Ficus caricaL, also known as pre-treatment.Ficus caricaL is the very important step of metatitanic acid, and metatitanic acid is not if carried out Ficus caricaL and directly calcination, and the product particle obtained is often very hard, form and aspect and other pigment performances very poor, paint poor performance.Ficus caricaL step additive used has a lot, and such as sylvite, microcosmic salt, aluminium salt etc., they are the negative contact agent of rutile-type mostly.
The present invention regulates and controls calcination process by adding microcosmic salt, sylvite, aluminium salt and antimonic salt in metatitanic acid successively, improves the sunproof object of titanium dioxide, also do not affect the conversion of rutile-type simultaneously to reach.Salt treatment agent formula of the present invention be cooperatively interact, complementary, if only separately add wherein one or both salts, do not reach ideal effect.As a small amount of P
2o
5the whiteness of product can be improved when calcining, making the good pulverizing of product softness; Sylvite can suppress the conversion rate of rutile-type, reduces calcining desulfurization temperature, avoid particles sintering to grow up; Aluminium salt can enter into the lattice of titanium dioxide, makes product particle fine and close, inherently improves the photostabilization of TiO 2 pigment; Simultaneously in order to the increase eliminating aluminium salts contg brings the problem of the yellow phase of titanium dioxide, the present invention adds additional sb oxide, adding of antimony compounds can make titanium dioxide be blue phase, and then the titanium dioxide making the present invention obtain can also keep very high whiteness in the performance with high-light-fastness, whiteness and photostabilization is made to obtain contradiction unified.But the add-on of these salt is also worthy of careful study, if add too much, then suppress the conversion of rutile-type, but add very few, then whiteness, weathering resistance do not reach ideal effect again.The present invention is drawn by a series of experiment: microcosmic salt addition is TiO
20.20%(with P
2o
5meter); Sylvite addition is TiO
20.27%(with K
2o counts); Dosage licked by aluminium salt is TiO
20.4-0.6%(with Al
2o
3meter); It is TiO that antimonic salt licks dosage
20.15%(with Sb
2o
3meter) time, the Rutile type Titanium Dioxide base material of excellent combination property, high whiteness and high-weatherability can be obtained.
Compared with prior art, the invention has the advantages that:
(1) pass through regulation and control Ficus caricaL formula in Ficus caricaL step, can realize the titanium dioxide product of high whiteness high-weatherability, simple to operate compared with coating method, method is more effective;
(2) in Ficus caricaL step, aluminium content is increased to 0. 4-0.8%, makes aluminium salt enter into lattice in titanium dioxide crystal growing process, thus improve the light fastness of TiO 2 pigment in essence;
(3) by introducing antimonic salt in Ficus caricaL process, eliminating aluminium content and improving the yellow phase problem brought, thus improving the whiteness of product;
(4) salt treatment agent formula of the present invention ensure that whiteness and the photostabilization of product, reduce between calcining temperature to 1050 DEG C ~ 1080 DEG C simultaneously and can obtain rutile titanium dioxide base material, avoid the too high impact that pigment performance is produced of calcining temperature, the product dispersing property obtained is good, whiteness is high, and photostabilization is strong.
Embodiment
In order to the object of the present invention of understanding clearly, technical scheme and beneficial effect, below the present invention is described further, but not by protection scope of the present invention limit in the examples below.
The preparation method of high whiteness light-fastness rutile type silicon dioxide substrate of the present invention, comprises the following steps:
(1) metatitanic acid is prepared: ilmenite and sulfuric acid solution obtain titanyl sulfate, generate metatitanic acid through sedimentation, crystallization, hydrolysis;
(2) metatitanic acid is once washed: the deionized water wash metatitanic acid by temperature being 50 ~ 80 DEG C, removes metallic impurity wherein;
(3) prepare metatitanic acid slurry: add water in the metatitanic acid after washing making beating, the concentration of slurry is 300 ~ 350g/L;
(4) bleach metatitanic acid slurry: in metatitanic acid slurry, add sulfuric acid, make the sulfuric acid concentration of slurry be 60 ~ 90g/L, and in slurry, add the rutile type calcining seeds of 5wt% and the Ti of 0.2wt% simultaneously
3+solution, weight percent metering benchmark is the total mass of titanium dioxide in metatitanic acid slurry, described Ti
3+the concentration of solution is 0.6g/L;
(5) metatitanic acid secondary washing: by the metatitanic acid slurry of reduction bleaching, filter with the leaf filter of negative pressure of vacuum or rotary vacuum drum filter midge, be the deionized water wash metatitanic acid of 50 ~ 80 DEG C again by temperature, wash away ferrous sulfate further, to reduce the content of iron, until the content of metatitanic acid ferrous ions is less than 20ppm;
(6) Ficus caricaL: add water the metatitanic acid after secondary washing making beating, and the concentration of slurry is 300 ~ 350g/L; The sb oxide of the potassium compound of 0.27wt%, the phosphorus compound of 0.2wt%, the aluminum compound of 0.4-0.8wt% and 0.15wt% is once added in metatitanic acid slurry, mix, its weight percent metering benchmark is two total masses of washing titanium dioxide in metatitanic acid slurry, and potassium compound add-on is with K
2o counts, and phosphorus compound add-on is with P
2o
5meter, aluminum compound add-on is with Al
2o
3meter, sb oxide add-on is with Sb
2o
3meter;
(6) calcining is pulverized: above-mentioned metatitanic acid de-watering of slurries calcining, calcining temperature controls between 1050 DEG C ~ 1080 DEG C, and after calcining, namely pulverizing obtains rutile titanium dioxide base material.
Illustrate with specific embodiment below:
Embodiment 1:
(1) prepare metatitanic acid slurry: get one washed after metatitanic acid, add enough deionized waters, being configured to slurry total mass is 2000g, TiO
2content is the metatitanic acid slurry of 25%;
(2) bleaching of metatitanic acid: slowly add the 90g vitriol oil, and stirred, is then heated to 60 DEG C in a water bath by system;
(3) add 5.0% calcining seeds, namely add the calcining seeds that 238.1g massfraction is 10.5%, after stirring 30min, add the Ti that 14g massfraction is 5.15%
3+solution, then continues to stir 90min;
(4) metatitanic acid after bleaching with the deionized water wash that temperature is 50-80 DEG C, then making beating is configured to the metatitanic acid slurry of 300g/L and carries out quantitative analysis to slurry, and its ferrous ion content is less than 20ppm;
(5) by 7.80g massfraction be 17.31% KOH(add rear K
2the massfraction of O is 0.27%), 4.20g massfraction is the H of 23.86%
3pO
4(add rear P
2o
5massfraction be 0.20%), 35.46g massfraction is the Al of 5.64%
2(SO
4)
3(add rear Al
2o
3massfraction be 0.40%) and the mixing of 0.75g antimonous oxide powder after add together in above-mentioned metatitanic acid slurry and mix;
(6) in retort furnace, be raised to 600 DEG C from room temperature in one hour after being dried by above-mentioned slurry, be then warming up to 1050 DEG C with 1 DEG C/min heat-up rate from 600 DEG C and namely obtain rutile titanium dioxide base material.
Embodiment 2:
(1) prepare metatitanic acid slurry: get one washed after metatitanic acid, add enough deionized waters, to be configured to slurry total mass be 2000g, TiO2 content be 25% metatitanic acid slurry;
(2) bleaching of metatitanic acid: slowly add the 90g vitriol oil, and stirred, is then heated to 60 DEG C in a water bath by system;
(3) add 5.0% calcining seeds, namely add the calcining seeds that 238.1g massfraction is 10.5%, after stirring 30min, add the Ti that 14g massfraction is 5.15%
3+solution, then continues to stir 90min;
(4) metatitanic acid after bleaching with the deionized water wash that temperature is 50-80 DEG C, then making beating is configured to the metatitanic acid slurry of 300g/L and carries out quantitative analysis to slurry, and its ferrous ion content is less than 20ppm;
(5) by 7.80g massfraction be 17.31% KOH(add rear K
2the massfraction of O is 0.27%), 4.20g massfraction is the H of 23.86%
3pO
4(add rear P
2o
5massfraction be 0.20%), 53.20g massfraction is the Al of 5.64%
2(SO
4)
3(add rear Al
2o
3massfraction be 0.60%) and the mixing of 0.75g antimonous oxide powder after add together in above-mentioned metatitanic acid slurry and mix;
(6) in retort furnace, be raised to 600 DEG C from room temperature in one hour after being dried by above-mentioned slurry, be then warming up to 1060 DEG C with 1 DEG C/min heat-up rate from 600 DEG C and namely obtain rutile titanium dioxide base material.
Embodiment 3:
(1) prepare metatitanic acid slurry: get one washed after metatitanic acid, add enough deionized waters, to be configured to slurry total mass be 2000g, TiO2 content be 25% metatitanic acid slurry;
(2) bleaching of metatitanic acid: slowly add the 90g vitriol oil, and stirred, is then heated to 60 DEG C in a water bath by system;
(3) add 5.0% calcining seeds, namely add the calcining seeds that 238.1g massfraction is 10.5%, after stirring 30min, add the Ti3+ solution that 14g massfraction is 5.15%, then continue to stir 90min;
(4) metatitanic acid after bleaching with the deionized water wash that temperature is 50-80 DEG C, then making beating is configured to the metatitanic acid slurry of 300g/L and carries out quantitative analysis to slurry, and its ferrous ion content is less than 20ppm;
(5) by 7.80g massfraction be 17.31% KOH(add rear K
2the massfraction of O is 0.27%), 4.20g massfraction is the H of 23.86%
3pO
4(add rear P
2o
5massfraction be 0.20%), 70.92g massfraction is the Al of 5.64%
2(SO
4)
3(add rear Al
2o
3massfraction be 0.40%) and the mixing of 0.75g antimonous oxide powder after add together in above-mentioned metatitanic acid slurry and mix;
(6) in retort furnace, be raised to 600 DEG C from room temperature in one hour after being dried by above-mentioned slurry, be then warming up to 1080 DEG C with 1 DEG C/min heat-up rate from 600 DEG C and namely obtain rutile titanium dioxide base material.
Comparative example:
Step, with embodiment 3, just only adds the Al that 44.33g massfraction is 5.64% in step (5)
2(SO
4)
3(add rear Al
2o
3massfraction be 0.25%), step (6) calcining temperature is changed accordingly.
Shown in each embodiment experimental result sees the following form:
As can be seen from the above table, with the rutile titanium dioxide base material that the inventive method is obtained, not only every quality index is better, and photostabilization obtains and significantly improves.The present invention adopts the obtained rutile titanium dioxide increasing aluminium salt to maintain very high dry powder whiteness, does not affect other pigment performances simultaneously.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments, equivalent and improve done in the spirit and principles in the present invention, are all included in of the present invention comprising within scope.
Claims (7)
1. a preparation method for high whiteness light-fastness rutile type silicon dioxide substrate, comprises metatitanic acid and once washes, prepares metatitanic acid slurry, bleaching metatitanic acid slurry, the washing of metatitanic acid secondary, Ficus caricaL and calcining pulverising step, it is characterized in that:
(1) in described bleaching metatitanic acid slurry stage, in slurry, the rutile type calcining seeds of 5wt% and the Ti of 0.2wt% is added
3+solution, weight percent metering benchmark is the total mass of titanium dioxide in metatitanic acid slurry, described Ti
3+the concentration of solution is 0.6g/L;
(2) described Ficus caricaL step is the sb oxide once adding the potassium compound of 0.27wt%, the phosphorus compound of 0.2wt%, the aluminum compound of 0.4-0.8wt% and 0.15wt% in the metatitanic acid after secondary washing, mix, its weight percent metering benchmark is two total masses of washing titanium dioxide in metatitanic acid slurry, and potassium compound add-on is with K
2o counts, and phosphorus compound add-on is with P
2o
5meter, aluminum compound add-on is with Al
2o
3meter, sb oxide add-on is with Sb
2o
3meter;
(3) in described calcining pulverising step, calcining temperature controls between 1050 DEG C ~ 1080 DEG C.
2. the preparation method of a kind of high whiteness light-fastness rutile type silicon dioxide substrate according to claim 1, is characterized in that: it is be the deionized water wash metatitanic acid of 50 ~ 80 DEG C by temperature that described metatitanic acid is once washed with the method for secondary washing.
3. the preparation method of a kind of high whiteness light-fastness rutile type silicon dioxide substrate according to claim 1, is characterized in that: the content that described metatitanic acid secondary washing retrodeviates metatitanic acid ferrous ions should be less than 20ppm.
4. the preparation method of a kind of high whiteness light-fastness rutile type silicon dioxide substrate according to claim 1, is characterized in that: described potassium compound is selected from potassium hydroxide, salt of wormwood and saltpetre.
5. the preparation method of a kind of high whiteness light-fastness rutile type silicon dioxide substrate according to claim 1, is characterized in that: described phosphorus compound is selected from phosphoric acid, Sodium hexametaphosphate 99 and ammonium phosphate.
6. the preparation method of a kind of high whiteness light-fastness rutile type silicon dioxide substrate according to claim 1, is characterized in that: described aluminum compound is selected from Tai-Ace S 150, aluminum chloride and sodium metaaluminate.
7. the preparation method of a kind of high whiteness light-fastness rutile type silicon dioxide substrate according to claim 1, is characterized in that: described sb oxide is antimonous oxide.
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Address after: 441500 No.1 Bianhe Road, Chengguan Town, Nanzhang County, Xiangyang City, Hubei Province Patentee after: Longbai Xiangyang Titanium Industry Co.,Ltd. Address before: 441500 No.1 Bianhe Road, Chengguan Town, Nanzhang County, Xiangyang City, Hubei Province Patentee before: XIANGYANG LOMON TITANIUM INDUSTRY Co.,Ltd. |