CN110467218A - The method for bleaching of metatitanic acid in a kind of Titanium White Production By Sulfuric Acid Process - Google Patents
The method for bleaching of metatitanic acid in a kind of Titanium White Production By Sulfuric Acid Process Download PDFInfo
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- CN110467218A CN110467218A CN201910892633.0A CN201910892633A CN110467218A CN 110467218 A CN110467218 A CN 110467218A CN 201910892633 A CN201910892633 A CN 201910892633A CN 110467218 A CN110467218 A CN 110467218A
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- metatitanic acid
- bleaching
- titanium dioxide
- dioxide
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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
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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
Abstract
The present invention relates to a kind of method for bleaching of metatitanic acid in Titanium White Production By Sulfuric Acid Process, the method for bleaching includes the following steps: that (1) weighs metatitanic acid slurry, spare;(2) water is added into metatitanic acid slurry, stirs evenly, thiourea dioxide is then added, heating while stirring makes sufficiently to react, after, it is successively filtered, washes, the metatitanic acid after being bleached.Method for bleaching of the present invention is compared with traditional method for bleaching using sulfuric acid dissolution, titanous reduction, iron tramp removal rate is high, and the pigment performance for the titanium dioxide being finally prepared is excellent, and operation of the present invention is simple, wide in range to process conditions requirement, low production cost reduces waste discharge.
Description
Technical field
The invention belongs to titanium white production technical fields, and in particular to the drift of metatitanic acid in a kind of Titanium White Production By Sulfuric Acid Process
Whitening method.
Background technique
Titanium dioxide (being commonly called as titanium dioxide) is a kind of white pigment optimal so far, and titanium dioxide is nontoxic, physical chemistry
Property is sufficiently stable, is a kind of pigment with excellent optical performance.In sulfuric acid method titanium pigment production technology, washing retrodeviates titanium
Extension of the trace iron tramp with washing time, the reduction of acidity in acid, are gradually oxidized in the form of solid hydroxide high-speed rail
In the presence of chemical reaction is as follows: 4FeSO4+O2+2H2SO4=====2Fe2(SO4)3+2H2O;
Fe2(SO4)3+6H2O=====2Fe (OH)3↓+3H2O (as PH >=1.5)
The Fe (OH) of generation3It not can be removed by washing, be converted into Fe203Content applies production 0.01% or more
For material titanium dioxide, it will highly impact the whiteness of titanium dioxide.In addition, in metatitanic acid Trace Iron after high-temperature calcination,
Generate red Fe203Reduce form and aspect, while Fe203It is mixed into rutile lattice, causes lattice deformability, causes lattice defect, shape
Lead to the decline of whiteness and reducing power to improve the light absorption energy of product at color development activation point, influences the light of titanium dioxide
Learn property.Make rutile titanium white powder that yellow be presented.Method general at present is to use sulfuric acid dissolution, is then gone back with titanous
Original makes Fe203Content can be reduced to 0.003% and significantly mention hereinafter, having the whiteness of finished product titanium dioxide obtained and glossiness
It is high.Its chemical reaction is as follows:
2Fe(OH)3+3H2SO4====Fe2(SO4)3+6H2O;
Fe2(SO4)3+Ti2(SO4)3+6H2O===2FeSO4+2TiOSO4+2H2SO4
But time-consuming, at high cost for this method for bleaching restored using sulfuric acid dissolution and titanous, the titanium finally prepared
The pigment performance of white powder is still less desirable, and causes the sewage discharge of relatively large dilute sulfuric acid and aluminium element.
Summary of the invention
In order to solve the above-mentioned problems in the prior art, the present invention provides inclined titanium in a kind of Titanium White Production By Sulfuric Acid Process
The method for bleaching of acid.The energy-saving and emission-reduction that the method advocates current country have good exemplary role, while this method is grasped
Make simply, wide in range to process conditions requirement, iron tramp removal rate is high, and the pigment performance for the titanium dioxide being prepared is excellent, and big
Width reduces production cost.
The technical solution of the present invention is as follows:
The method for bleaching of metatitanic acid, includes the following steps: in a kind of Titanium White Production By Sulfuric Acid Process
(1) metatitanic acid slurry is weighed, it is spare;
(2) water is added into metatitanic acid slurry, stirs evenly, thiourea dioxide is then added, heating while stirring makes to fill
Divide reaction, after, it is successively filtered, washes, the metatitanic acid after being bleached.
Thiourea dioxide, No. CAS: 1758-73-2 or 4189-44-0, molecular formula: CH4N2O2S, molecular weight: 108.12, in
Literary alias: methyl sulfinate, formamidinesulfinic acid, white crystals particle, non-toxic and tasteless, density: 2.25g/cm3, fusing point: 126 DEG C, boiling
Point: 355.3 DEG C of at 760mmHg, refractive index: 1.66, flash-point: 168.7 DEG C.With reduction potential is high, thermal stability is good, storage
The features such as convenient transportation, be widely used in the dyeing of reducing dye and sulfur dye, the bleaching of wool silk, disperse dyes also
Original cleaning, directly or the stripping of the bad dyeing of reactive dye, the cleaning of dye vat etc..In addition, being also applied to paper pulp in paper industry
Bleaching, the deinking of waste paper etc.;It is used as catalyst, the stabilizer of synthetic resin in Macromolecular materials industry, in organic synthesis
The fine chemistry industries such as photosensitive material, medicament, medicine, fragrance.
Preferably, in step (2), the concentration that titanium dioxide in metatitanic acid slurry is added water to described in progress is 180-320g/
L。
Preferably, the concentration that titanium dioxide in metatitanic acid slurry is added water to described in progress is 280g/L.
Preferably, in step (2), the additional amount of the thiourea dioxide is titanium dioxide quality in metatitanic acid slurry
0.3-0.6%.
Preferably, the additional amount of the thiourea dioxide is 0.4% of titanium dioxide quality in metatitanic acid slurry.
Preferably, in step (2), the temperature of the heating is 40-70 DEG C, and the speed of the stirring is 1000-2000r/
Min, the time of the stirring are 15-40min.
Preferably, the temperature of the heating is 50 DEG C, and the speed of the stirring is 1500r/min, the time of the stirring
For 30min.
Preferably, in step (2), the washing is to be washed using washing diaphragm filter press.
Preferably, in step (2), the temperature of the washing is 40-60 DEG C.
Application of the thiourea dioxide in the reducing agent for being used to prepare titanium dioxide bleaching.
The invention has the benefit that
The method for bleaching of metatitanic acid in Titanium White Production By Sulfuric Acid Process of the present invention, using thiourea dioxide as reducing agent,
By with existing Fe in solid form in metatitanic acid3+, i.e. Fe (OH)3Reaction makes it be converted into water-soluble Fe2+, pass through washing
It removes, to achieve the purpose that iron impurity.The method that the present invention uses thiourea dioxide to be bleached, it is molten with use sulfuric acid
Traditional method for bleaching of solution, titanous reduction is compared, and iron tramp removal rate is high, the pigment performance for the titanium dioxide being finally prepared
It is excellent, and operation of the present invention is simple, wide in range to process conditions requirement, low production cost reduces waste discharge.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, technical solution of the present invention will be carried out below
Detailed description.Obviously, described embodiment is only a part of the embodiments of the present invention, instead of all the embodiments.
Based on the embodiments of the present invention, those of ordinary skill in the art obtained institute without making creative work
There is other embodiment, belongs to the range that the present invention is protected.
Embodiment 1
The present embodiment provides a kind of method for bleaching of metatitanic acid in Titanium White Production By Sulfuric Acid Process, include the following steps:
(1) metatitanic acid slurry is weighed, it is spare;
(2) water is added into metatitanic acid slurry, the concentration for adjusting titanium dioxide in metatitanic acid slurry is 180g/L, and stirring is equal
It is even, the thiourea dioxide for accounting for titanium dioxide quality 0.3% in metatitanic acid slurry is then added, being heated to temperature is 40 DEG C, simultaneously
Make sufficiently to react with the mixing speed stirring 40min of 1000r/min, after, it is successively filtered, washes diaphragm filter press 40
DEG C water washing, the metatitanic acid after being bleached.
Embodiment 2
The present embodiment provides a kind of method for bleaching of metatitanic acid in Titanium White Production By Sulfuric Acid Process, include the following steps:
(1) metatitanic acid slurry is weighed, it is spare;
(2) water is added into metatitanic acid slurry, the concentration for adjusting titanium dioxide in metatitanic acid slurry is 320g/L, and stirring is equal
It is even, the thiourea dioxide for accounting for titanium dioxide quality 0.6% in metatitanic acid slurry is then added, being heated to temperature is 70 DEG C, simultaneously
Make sufficiently to react with the mixing speed stirring 15min of 2000r/min, after, it is successively filtered, washes diaphragm filter press 60
DEG C water washing, the metatitanic acid after being bleached.
Embodiment 3
The present embodiment provides a kind of method for bleaching of metatitanic acid in Titanium White Production By Sulfuric Acid Process, include the following steps:
(1) metatitanic acid slurry is weighed, it is spare;
(2) water is added into metatitanic acid slurry, the concentration for adjusting titanium dioxide in metatitanic acid slurry is 280g/L, and stirring is equal
It is even, the thiourea dioxide for accounting for titanium dioxide quality 0.4% in metatitanic acid slurry is then added, being heated to temperature is 50 DEG C, simultaneously
Make sufficiently to react with the mixing speed stirring 30min of 1500r/min, after, it is successively filtered, washes diaphragm filter press 50
DEG C water washing, the metatitanic acid after being bleached.
Comparative example 1
Difference with embodiment 3, which is only that, replaces with sodium bisulphite formaldehyde for thiourea dioxide.
Comparative example 2
Difference with embodiment 3, which is only that, replaces with zinc sulfite for thiourea dioxide.
Comparative example 3
It conventionally carries out except iron, specifically, this comparative example provides metatitanic acid in a kind of Titanium White Production By Sulfuric Acid Process
Method for bleaching, include the following steps:
(1) metatitanic acid slurry is weighed, it is spare;
(2) water is added into metatitanic acid slurry, the concentration for adjusting titanium dioxide in metatitanic acid slurry is 280g/L, and stirring is equal
It is even, 60mL sulfuric acid is then sequentially added, 3mL trivalent titanium solution, being heated to temperature is 50 DEG C, while with the stirring of 1500r/min
Speed stirring 30min makes sufficiently to react, after, it is successively filtered, the water washing of 50 DEG C of diaphragm filter press of washing is floated
Metatitanic acid after white.
Test example
1, the experimental study of de-ferrous effect of the present invention
Metatitanic acid after bleaching that 1-3 of the embodiment of the present invention and comparative example 1-3 are prepared is carried out drying and dewatering to take off
After sulphur, the contrast test of titanium white powder pigment performance is carried out, while having carried out the method for the present invention (embodiment 3) and conventional method is (right
Ratio 3) cost analysis, the results are shown in Table 1,2.
Wherein, L*, a*, b* are except the data after iron, L0、a0、b0For except the data before iron;L represents brightness, and numerical value is bigger,
Indicate that brightness is bigger;A indicates green to the variation tendency between red, and numerical value is bigger closer to red, smaller closer to green;
B indicates yellow to the variation tendency of blue, and numerical value is bigger closer to yellow, smaller closer to blue;Wr represents Blue Whiteness, Wh
Hunter whiteness is represented, numerical value is bigger to indicate whiter.
1 metatitanic acid of table is except color characteristics comparison before and after iron
2 Cost comparisons of table
The result shows that the pigment performance for the metatitanic acid that method for bleaching of the present invention is prepared is substantially better than comparative example 1-3, say
Its bright de-ferrous effect is more preferable, meanwhile, method for bleaching of the present invention is compared with the traditional method, and significantly reduces production cost.
2, the experimental study of thiourea dioxide additive amount
A certain amount of metatitanic acid is placed in a beaker, adding water to adjust the concentration of titanium dioxide is 283g/L, respectively according to two
Thiourea dioxide is added in 0.3%, 0.4%, 0.5%, 0.6% additive amount of titanium oxide quality, and being heated to temperature is 55 DEG C, together
When make sufficiently to react with the revolving speed of 1500r/min stirring 30min, after filter, washed with 800mL50 DEG C of distilled water
It washs, after filter cake drying and dewatering desulfurization, carries out the contrast test analysis of impurity content and titanium dioxide color characteristics, while doing sky
White test.
Test result is as shown in Table 3 and Table 4, the results showed that under conditions of concentration, temperature, revolving speed are certain, sulfur dioxide
When the additive amount of urea is the 0.4% of titanium dioxide quality, de-ferrous effect and economic cost are best.
3 metatitanic acid thiourea dioxide method of table is except chemical component before and after iron
4 metatitanic acid thiourea dioxide method of table is except color characteristics before and after iron
3, the experimental study of thiourea dioxide reaction temperature
A certain amount of metatitanic acid is placed in a beaker, adding water to adjust the concentration of titanium dioxide is 283g/L, according to titanium dioxide
Thiourea dioxide is added in 0.4% additive amount of titanium quality, and the temperature of reaction system is set as 1#:40 DEG C respectively;2#:50
℃;3#:60 DEG C;4#:70 DEG C of progress condition test, while making sufficiently to react with the revolving speed of 1500r/min stirring 30min, it finishes
After filter, washed with 800mL50 DEG C of distilled water, after filter cake drying and dewatering desulfurization, carry out impurity content and titanium white
The contrast test of powder color characteristics is analyzed, while doing blank test.
Test result is as shown in table 5 and table 6, the results showed that when the certain item of concentration, the dosage of thiourea dioxide, revolving speed
Under part, when the temperature of reaction system is 50 DEG C, de-ferrous effect is best.
5 metatitanic acid thiourea dioxide method of table is except chemical component before and after iron
6 metatitanic acid thiourea dioxide method of table is except color characteristics before and after iron
4, in metatitanic acid titanium dioxide concentration experimental study
A certain amount of metatitanic acid is placed in a beaker, adding water to adjust the concentration of titanium dioxide respectively is 1#:180g/L;2#:
240g/L;3#:280g/L;4#:320g/L carries out condition test, is added two according to 0.4% additive amount of titanium dioxide quality
Aminoiminomethanesulfonic acid, be heated to temperature be 50 DEG C, while with the revolving speed of 1500r/min stirring 30min make sufficiently to react, after mistake
Filter, is washed with 800mL50 DEG C of distilled water, after filter cake drying and dewatering desulfurization, carries out impurity content and titanium dioxide face
The contrast test of color performance is analyzed, while doing blank test.
Test result is as shown in table 7 and table 8, the results showed that when the certain item of temperature, the dosage of thiourea dioxide, revolving speed
Under part, when titanium dioxide concentration is 280g/L in metatitanic acid, de-ferrous effect is best.
7 metatitanic acid thiourea dioxide method of table is except chemical component before and after iron
8 metatitanic acid thiourea dioxide method of table is except color characteristics before and after iron
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
Those familiar with the art in the technical scope disclosed by the present invention, can easily think of the change or the replacement, and should all contain
Lid is within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.
Claims (10)
1. the method for bleaching of metatitanic acid in a kind of Titanium White Production By Sulfuric Acid Process, which comprises the steps of:
(1) metatitanic acid slurry is weighed, it is spare;
(2) water is added into metatitanic acid slurry, stirs evenly, thiourea dioxide is then added, heating while stirring, it is sufficiently anti-to make
It answers, after, it is successively filtered, washes, the metatitanic acid after being bleached.
2. the method according to claim 1, wherein being added water to described in progress in metatitanic acid slurry in step (2)
The concentration of titanium dioxide is 180-320g/L.
3. according to the method described in claim 2, it is characterized in that, adding water to titanium dioxide in metatitanic acid slurry described in carrying out
Concentration is 280g/L.
4. the method according to claim 1, wherein the additional amount of the thiourea dioxide is inclined in step (2)
The 0.3-0.6% of titanium dioxide quality in metatitanic acid slurry.
5. according to the method described in claim 4, it is characterized in that, the additional amount of the thiourea dioxide is in metatitanic acid slurry
The 0.4% of titanium dioxide quality.
6. the method according to claim 1, wherein the temperature of the heating is 40-70 DEG C, institute in step (2)
The speed for stating stirring is 1000-2000r/min, and the time of the stirring is 15-40min.
7. according to the method described in claim 6, it is characterized in that, the temperature of the heating be 50 DEG C, the speed of the stirring
For 1500r/min, the time of the stirring is 30min.
8. the method according to claim 1, wherein the washing is using washing diaphragm filters pressing in step (2)
Machine is washed.
9. the method according to claim 1, wherein the temperature of the washing is 40-60 DEG C in step (2).
10. application of the thiourea dioxide in the reducing agent for being used to prepare titanium dioxide bleaching.
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Cited By (3)
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CN111054398A (en) * | 2019-12-23 | 2020-04-24 | 安徽迪诺环保新材料科技有限公司 | Raw material for preparing flue gas denitration catalyst by using molybdenum trioxide, catalyst and preparation method |
CN113929132A (en) * | 2021-09-24 | 2022-01-14 | 东华工程科技股份有限公司 | Sulfuric acid method titanium dioxide metatitanic acid bleaching method and system |
CN114213874A (en) * | 2021-12-03 | 2022-03-22 | 贵州民族大学 | Processing method for quality improvement and whitening of barite ore |
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CN114213874A (en) * | 2021-12-03 | 2022-03-22 | 贵州民族大学 | Processing method for quality improvement and whitening of barite ore |
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Application publication date: 20191119 |