CN101863508B - High-purity mixed-crystal titanium pigment and production method thereof - Google Patents
High-purity mixed-crystal titanium pigment and production method thereof Download PDFInfo
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- CN101863508B CN101863508B CN 201010184276 CN201010184276A CN101863508B CN 101863508 B CN101863508 B CN 101863508B CN 201010184276 CN201010184276 CN 201010184276 CN 201010184276 A CN201010184276 A CN 201010184276A CN 101863508 B CN101863508 B CN 101863508B
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Abstract
The invention discloses high-purity mixed-crystal titanium pigment and a production method thereof, which are applicable to the capacitor industry. The titanium pigment comprises the following components in percentage by weight: more than 99.5 percent of titanium dioxide, 25 to 85 percent of rutile-typed titanium pigment and 15 to 75 percent of anatase-typed titanium pigment. The method comprises the following steps: a. hydrolyzing the refined titanium sulfate to obtain hydrolysis metatitanic acid pulp; b. filtering the metatitanic acid pulp, utilizing the water with the electric conductivity being less than 100 microseconds per centimeter or with the pH value of 2 to 7 to wash the filter cake for 1 to 4 hours to obtain metatitanic acid for one time; c. roasting the obtained metatitanic acid at the temperature of 900 to 1200 DEG C, and then cooling and grinding the roasted metatitanic acid to obtain a finshed product. Compared with the prior art, the method has the advantages that the quality and the application stability of the capacitor can be improved, the water can be saved, the loss of titanium dioxide can be reduced, the production cost can be reduced, the process is simple, the operation is convenient, the control is convenient, industrialized production can be realized, and the like.
Description
Technical field
The invention belongs to chemical production field, a kind of specifically high-purity mixed-crystal titanium pigment and working method thereof, it is particularly useful for the electrical condenser industry.
Background technology
White titanium pigment is one of most important mineral dye and industrial chemicals, as a kind of opaque pigment, is widely used in industries such as coating, papermaking, plastics, rubber, rubber-emulsion paint, printing-ink, chemical fibre; As a kind of industrial chemicals product, be mainly used in fields such as enamel, electrical condenser, metallurgy, welding electrode.At present, the method for producing white titanium pigment mainly comprises sulfuric acid process and chlorination, in the sulfuric acid method titanium pigment actual production process of this area, generally adopts secondary water washing about producing the high-purity titanium white powder; Titanium oxide purity only reaches 99.0%, and crystalline structure is an anatase titanium dioxide, and it is low to exist resistance value when being used for electrical condenser; Electrical condenser is prone to unsteady phenomenon when using, and adopts secondary water washing, and washing total time is at 4-6h; Water consumption is big, and titanium oxide runs off and increases, and consuming increases.Like application number is that 200810070681 Chinese invention patent discloses name and is called " preparation method of high pure macroparticle anatase type titanium dioxide "; This invented technology for " 0.5～2 gram titanium oxide and concentration is that alkaline solution thorough mixing in stainless steel autoclave or polytetrafluoroethylcontainer container of 40～60 milliliter of 10～15 mol is even, and mixture reacts 60～100h under 453～493K; The product p H value that generates is adjusted to 9～11; Being placed in stainless steel autoclave or the polytetrafluoroethylcontainer container reacts after 2～3 days under 453～493K again; Behind the zero(ppm) water thorough washing, constant pressure and dry 1～40h obtains final high pure macroparticle anatase type titanium dioxide under 323～373K." this method adopt the industriallization titanium white production finished product as raw material, cost increases, and adopts high-tension apparatus, reaction time is long, production capacity is low, is unfavorable for industrialized production.And the product of producing only contains the Detitanium-ore-type crystal formation, does not reach the requirement that electrical condenser is produced.
Summary of the invention
The present invention is directed to deficiency of the prior art; A kind of high-purity mixed-crystal titanium pigment is provided; This white titanium pigment comprises the white titanium pigment of two types of Rutile type Titanium Dioxide and anatase thpe white powders, is applied to the electrical condenser industry, can improve the quality and the electrical condenser stability in use ability of electrical condenser.
In order to solve the problems of the technologies described above, the present invention is able to solve through following technical proposals:
A kind of high-purity mixed-crystal titanium pigment; By weight percentage: the content of titanium oxide is greater than 99.5%, and includes Rutile type Titanium Dioxide and anatase thpe white powder simultaneously, wherein; The content of Rutile type Titanium Dioxide is 25% to 85%, and the content of anatase thpe white powder is 15% to 75%.
The content of Fe is less than 25ppm, and the content of S is less than 200ppm.
Another object of the present invention provides a kind of method of producing above-mentioned white titanium pigment:
A kind of working method of high-purity mixed-crystal titanium pigment may further comprise the steps:
A, purified titanium sulfate liquid is made hydrolysis metatitanic acid slurries after hydrolysis;
B, step a gained metatitanic acid slurries are filtered, and adopt specific conductivity to obtain metatitanic acid less than 100 μ s/cm or pH value for the water of 2-2.5 washs 1-4h to filter cake, said washing is once to wash;
C, step b gained metatitanic acid is calcined under 900-1200 ℃ temperature, then through cooling, get product after grinding.
Preferably, the specific conductivity described in the step b is through the de-salted water of sun bed resin, cloudy bed resins exchange or through the de-salted water of sun bed resin, the exchange of cloudy bed resins exchange regulating YIN and YANG mixed-bed resin less than the water of 100 μ s/cm.
Preferably, the pH value described in the step b is the sand leaching water of regulating with acid for the water of 2-2.5, and used acid is one or more in sulfuric acid, the hydrochloric acid.
Preferably, the iron titanium ratio of the purified titanium sulfate liquid described in the step a is 0.26 to 0.28, the F value is 1.84 to 1.86, titanous is that 1.3g/L to 1.7g/L, clarity are that one-level, stability are greater than 350mL, with TiO
2Meter, required concentration is 130g/L to 160g/L.
Further improve and comprise: the water that is used to wash said filter cake among the step b need reclaim the filtrating that washing finishes in preceding 0.5 hour, and the filtrating of this recovery is used for preceding 0.5 hour of next round filter cake washing.
Preferably, the calcining described in the step c is meant that in Φ 2400, Φ 2600, Φ 2800, Φ 3000, Φ 3200 or Φ 3600 rotary kilns, adopting fuel is that diesel oil, coal gas, liquefied gas or Sweet natural gas are calcined.
Preferably, the metatitanic acid of step b gained residence time in said rotary kiln is 8-16 hour, and calcining temperature is meant from 4 meters measured temperature values of temperature survey point of blanking port.
The present invention compared with prior art has following beneficial effect:
1) produce high-purity mixed-crystal titanium pigment, be applied to the electrical condenser industry, can improve electrical condenser quality and electrical condenser stability in use can;
2) adopt once washing, water saving, and reduced the loss of titanium oxide, reduced production cost;
3) technology is simple, and is easy to operate, is convenient to control, helps industrialized production.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is described in further detail:
Instance 1
With TiO
2Meter adopts method commonly used in the sulfuric acid method titanium pigment production process of this area to carry out the direct carbonated drink of normal pressure total titanium concentration POV titanium liquid that is 130g/L and separates, make hydrolysis metatitanic acid slurry; An employing mole leaf filter vacuum attraction filters again, behind the formation 3.5cm filter cake leaf filter is moved into washing bath and begins washing, and washing water employing salt acid for adjusting pH value is 2.5 sand leaching water; Behind the washing 1.5h wash filtrate is switched to the reuse tank, washing reaches 2h, and washing finishes; The gained metatitanic acid is sent into rotary kiln, stopped 12 hours at rotary kiln, control falls the kilneye temperature 1200 ℃ of calcinings; Cooling, grinding promptly get.
Instance 2
With TiO
2Meter adopts method commonly used in the sulfuric acid method titanium pigment production process of this area to carry out the direct carbonated drink of normal pressure total titanium concentration POV titanium liquid that is 140g/L and separates, make hydrolysis metatitanic acid slurry; An employing mole leaf filter vacuum attraction filters again, behind the formation 3.5cm filter cake leaf filter is moved into washing bath and begins washing, and washing water employing sulphur acid for adjusting pH value is 2.5 sand leaching water; Behind the washing 2h wash filtrate is switched to the reuse tank, washing reaches 2.5h, and washing finishes; The gained metatitanic acid is sent into rotary kiln, stopped 10 hours at rotary kiln, control falls the kilneye temperature 1100 ℃ of calcinings; Cooling, grinding promptly get.
Instance 3
With TiO
2Meter adopts method commonly used in the sulfuric acid method titanium pigment production process of this area to carry out the direct carbonated drink of normal pressure total titanium concentration POV titanium liquid that is 150g/L and separates, make hydrolysis metatitanic acid slurry; An employing mole leaf filter vacuum attraction filters again, behind the formation 3.5cm filter cake leaf filter is moved into washing bath and begins washing, and washing water elder generation is with the water washing 0.5h of reuse tank; Adopting the salt acid for adjusting pH value again is 2.5 sand leaching water, behind the washing 1.5h wash filtrate is switched to the reuse tank, and washing reaches 3h; Washing finishes, and the gained metatitanic acid is sent into rotary kiln, stops 10 hours at rotary kiln; Control falls the kilneye temperature 1150 ℃ of calcinings, and cooling, grinding promptly get.
Instance 4
With TiO
2Meter adopts method commonly used in the sulfuric acid method titanium pigment production process of this area to carry out the direct carbonated drink of normal pressure total titanium concentration POV titanium liquid that is 150g/L and separates, make hydrolysis metatitanic acid slurry; An employing mole leaf filter vacuum attraction filters again, behind the formation 3.5cm filter cake leaf filter is moved into washing bath and begins washing, and washing water elder generation is with the water washing 0.5h of reuse tank; After adopting de-salted water washing 1.5h again wash filtrate is switched to the reuse tank, washing reaches 2.5h, and washing finishes; The gained metatitanic acid is sent into rotary kiln, stopped 10 hours at rotary kiln, control falls the kilneye temperature 1150 ℃ of calcinings; Cooling, grinding promptly get.
Instance 5
With TiO
2Meter adopts method commonly used in the sulfuric acid method titanium pigment production process of this area to carry out the direct carbonated drink of normal pressure total titanium concentration POV titanium liquid that is 160g/L and separates, make hydrolysis metatitanic acid slurry; An employing mole leaf filter vacuum attraction filters again, behind the formation 3.5cm filter cake leaf filter is moved into washing bath and begins washing, and washing water elder generation is with the water washing 0.5h of reuse tank; After adopting de-salted water washing 2h again wash filtrate is switched to the reuse tank, washing reaches 3h, and washing finishes; The gained metatitanic acid is sent into rotary kiln, stopped 10 hours at rotary kiln, control falls the kilneye temperature 1100 ℃ of calcinings; Cooling, grinding promptly get.
Claims (7)
1. high-purity mixed-crystal titanium pigment; It is characterized in that: by weight percentage: the content of titanium oxide is greater than 99.5%; And include Rutile type Titanium Dioxide and anatase thpe white powder simultaneously; Wherein, the content of Rutile type Titanium Dioxide is 25% to 85%, and the content of anatase thpe white powder is 15% to 75%; It makes through following steps:
A, purified titanium sulfate liquid is made hydrolysis metatitanic acid slurries after hydrolysis; The iron titanium ratio of said purified titanium sulfate liquid is 0.26 to 0.28, the F value is 1.84 to 1.86, titanous is that 1.3g/L to 1.7g/L, clarity are that one-level, stability are greater than 350mL, with TiO
2Meter, required concentration is 130g/L to 160g/L;
B, step a gained metatitanic acid slurries are filtered, and adopt specific conductivity to obtain metatitanic acid less than 100 μ s/cm or pH value for the water of 2-2.5 washs 1-4h to filter cake, said washing is once to wash;
C, step b gained metatitanic acid is calcined under 900-1200 ℃ temperature, then through cooling, get product after grinding.
2. a kind of high-purity mixed-crystal titanium pigment according to claim 1 is characterized in that: the content of Fe is less than 25ppm, and the content of S is less than 200ppm.
3. a kind of high-purity mixed-crystal titanium pigment according to claim 1 is characterized in that: the specific conductivity described in the step b is through the de-salted water of sun bed resin, cloudy bed resins exchange or through the de-salted water of sun bed resin, the exchange of cloudy bed resins exchange regulating YIN and YANG mixed-bed resin less than the water of 100 μ s/cm.
4. a kind of high-purity mixed-crystal titanium pigment according to claim 1 is characterized in that: the pH value described in the step b is the sand leaching water of regulating with acid for the water of 2-2.5, and used acid is one or more in sulfuric acid, the hydrochloric acid.
5. according to claim 3 or 4 described a kind of high-purity mixed-crystal titanium pigments; It is characterized in that: the water that is used to wash said filter cake among the step b need reclaim the filtrating that washing finishes in preceding 0.5 hour, and the filtrating of this recovery is used for preceding 0.5 hour of next round filter cake washing.
6. a kind of high-purity mixed-crystal titanium pigment according to claim 5 is characterized in that: the calcining described in the step c is meant that in Φ 2400, Φ 2600, Φ 2800, Φ 3000, Φ 3200 or Φ 3600 rotary kilns, adopting fuel is that diesel oil, coal gas, liquefied gas or Sweet natural gas are calcined.
7. a kind of high-purity mixed-crystal titanium pigment according to claim 6 is characterized in that: the metatitanic acid of step b gained residence time in said rotary kiln is 8-16 hour, and calcining temperature is meant from 4 meters measured temperature values of temperature survey point of blanking port.
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| CN102390865B (en) * | 2011-08-11 | 2013-07-31 | 四川龙蟒钛业股份有限公司 | Method for preparing high-activity double-effect seed crystals from metatitanic acid |
| CN103043715B (en) * | 2012-12-19 | 2014-04-23 | 攀枝花鼎星钛业有限公司 | Production method of titanium dioxide powder |
| CN103708538B (en) * | 2013-12-20 | 2016-03-09 | 攀枝花东方钛业有限公司 | A kind of preparation method of trivalent titanium solution |
| CN104477981B (en) * | 2014-12-11 | 2016-05-04 | 山东东佳集团股份有限公司 | The preparation method of high-purity titanium dioxide |
| CN114573021A (en) * | 2022-03-14 | 2022-06-03 | 淮安市鸿洋钛业有限公司 | High-purity mixed crystal titanium dioxide and production method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1156690A (en) * | 1996-12-06 | 1997-08-13 | 罗孝良 | Method for manufacturing rutile type high-purity titanium dioxide |
| CN1814550A (en) * | 2006-03-03 | 2006-08-09 | 河北大学 | Method for preparing hano-level titanium dioxide by controlling crystal form |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1156690A (en) * | 1996-12-06 | 1997-08-13 | 罗孝良 | Method for manufacturing rutile type high-purity titanium dioxide |
| CN1814550A (en) * | 2006-03-03 | 2006-08-09 | 河北大学 | Method for preparing hano-level titanium dioxide by controlling crystal form |
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