CN1850619A - Method for preparing anatase chemical fiber special titanium pigment - Google Patents
Method for preparing anatase chemical fiber special titanium pigment Download PDFInfo
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- CN1850619A CN1850619A CN 200610040290 CN200610040290A CN1850619A CN 1850619 A CN1850619 A CN 1850619A CN 200610040290 CN200610040290 CN 200610040290 CN 200610040290 A CN200610040290 A CN 200610040290A CN 1850619 A CN1850619 A CN 1850619A
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- chemical fiber
- titanium dioxide
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- anatase
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Abstract
The invention is a method for preparing anatase chemical-fiber titanium dioxide, making acid hydrolysis with sulfuric acid, leaching and reducing, filtering the deposited titanium liquid and obtaining filtrate, freezing and crystallizing the filtrate to separate FeSO4 out, refiltering the filtrate and adding assistant crystal seeds into the second obtained filtrate for hydrolyzation, so as to separate out large amounts of metatitanic acid deposit and filtering out metatitanic acid solid; using metatitanic acid as raw material, processing the metatitanic acid into titanium oxysulfide thick titanium liquid with a certain F value by oil of vitriol, then processing deposit with salt, water washing and drying, calcining in rotary kiln, and crushing and making it, where the F value is controlled at 1.9 plus or minus 0.05, and the crystal seeds are added in 2.0 plus or minus 0.5% in the hydrolyzation course.
Description
Technical field
The present invention relates to the preparation method of titanium dioxide (titanium dioxide), especially the production method of chemical fibre anatase thpe white powder.
Background technology
The production method of a CN02121407.7 composite titanium dioxide, processing step comprises and the Calcined Kaolin from Coal Bearing Strata particle is carried out ultra tiny powder process, slurrying, hydrolysis coating, rinsing, crystallization roasting, a. slurrying: the suspension of the Calcined Kaolin from Coal Bearing Strata ultrafine powder being made concentration 10-30%; B. hydrolysis coating: heat when described suspension is stirred to 80-90 ℃, the inorganic titanium salts solution that adds 5-15% again carries out inorganic film-coating modification, and the pH value of the hierarchy of control is at 1.0-2.0.
The manufacture method of CN96117814.0 rutile type high-purity titanium dioxide, technical process has: after 1. ilmenite concentrate being pulverized, carry out 1～5 hour acidolysis reaction with the vitriol oil, add entry simultaneously and auxiliary agent reacts.2. in the acidolysis thing, add the reduction auxiliary agent, leach reduction 1-12 hour.3. add auxiliary agent and carried out sedimentation 1-24 hour in reduced liquid, the titanium liquid after the sedimentation gets filtered liquid through after filtering.4. after the filtered liquid freezing and crystallizing being separated out FeSO47H ↓ [2] O, filter to isolate green vitriol.5. the filtrate that filtrate is refiltered the back gained adds the auxiliary agent crystal seed and is hydrolyzed, and after treating to separate out the metatitanic acid throw out in a large number, filters out the metatitanic acid solid.6. wash the metatitanic acid solid with water, then metatitanic acid is carried out drying, calcining, pulverizing.
Technologies such as titanium dioxide carries out acidolysis with sulfuric acid process commonly used, and leaching is reduced, and the sedimentation filtering for crystallizing is separated, the pulverizing of hydrolysed filtrate washing drying and calcining and auxiliary agent are made.
CN1506311 nanometre-grade titanic-schorl type titanium dioxide powder preparation method, with the metatitanic acid is raw material, handle into the titanyl sulfate solution of certain F value with the vitriol oil, use the yellow soda ash neutralization precipitation again, wash this precipitation with water, use the hydrochloric acid peptization, the ammoniacal liquor gel, after filtration, prepared such as washing, dry, calcining and comminution by gas stream go out the nanometre-grade titanic-schorl type titanium dioxide powder.
Prior art does not have pair man-made fiber to do special explanation with the technology that is AH type anatase thpe white powder.
The sharp titanium titanium dioxide of chemical fibre is mainly used PET delustrant, and the Production Flow Chart of its production technique and anatase thpe white powder BA01-02 is similar, and its key is the control to particle diameter, and promptly size distribution is very narrow, and coarse particle and particulate subnumber are seldom; Dispersiveness and dispersion stabilization in water and hot ethylene glycol (for guaranteeing the polymeric quality of PET) are all fine, higher to the purity requirement of product in addition.As the TA-300 of Japan, its main technique is to have increased wet-milling and classification operation in the later stage.
Summary of the invention
The present invention seeks to: a kind of new preparation method that a kind of anatase chemical fiber titanium dioxide is provided, especially a kind of anatase thpe white powder of optimizing the several relevant significant parameter preparation of preparation process, have narrower particle size distribution, median size is moderate, the anatase chemical fiber titanium dioxide that performance is good.
The present invention seeks to realize like this: the anatase chemical fiber titanium dioxide the preparation method, sulfuric acid process is carried out acidolysis, the leaching reduction, the titanium liquid after the sedimentation is through after filtering, filtered liquid.The filtered liquid freezing and crystallizing is separated out FeSO
4, the filtrate adding auxiliary agent crystal seed that filtrate is refiltered the back gained is hydrolyzed, and separates out the metatitanic acid throw out in a large number and filters out the metatitanic acid solid; With the metatitanic acid is raw material, handles into the dense titanium liquid of titanyl sulfate of certain F value with the vitriol oil, handles precipitation with salt again, washes with water and drying, calcined by rotary kiln and pulverizing are prepared from.The F value of wherein controlling dense titanium liquid is 1.9 ± 0.05, especially 1.9 ± 0.02; An amount of crystal seed in the hydrolytic process, 2.0 ± 0.5%, especially 2.0 ± 0.2%, its unit is a weight ratio of being converted into titanium dioxide; The kiln temperature control condition of calcined by rotary kiln is: kiln hood: 960 ℃ ± 30 ℃, and kiln tail: 300 ℃ ± 15 ℃.
Salt is handled and can be adopted the alkali neutralization, by interpolation yellow soda ash, sodium hydroxide (potassium), or adopts simultaneously and adds following element:
P
2O
5%:0.18 ± 0.05, especially 0.18 ± 0.02
K
2O%:0.38 ± 0.05, especially 0.38 ± 0.02
Improvement of the present invention comprises: and salt control P when handling
2O
5/ K
2The ratio of O and be suitably to improve salt treatment agent total amount is adjusted calcining temperature and inlet amount, during pulverizing by adjusting machine speed.Wherein the F value refers to mH
2SO
4/ mTiO
2Ratio.
The present invention is a kind of new preparation method who is adapted to practicality of anatase chemical fiber titanium dioxide, control, optimize the several relevant significant parameter of preparation process on its technology by strictness: the F value that comprises dense titanium liquid, an amount of crystal seed in the hydrolytic process, and the ratio of salt control P2O5/K2O when handling and be suitably to improve salt treatment agent total amount, adjust calcining temperature and inlet amount, pass through to adjust the analytical engine machine speed during pulverizing.Zhi Bei anatase thpe white powder has narrower particle size distribution like this, and median size is moderate, and its pigment performance and particle property can satisfy the production needs of chemical fibre titanium.The key technical indexes is:
| Project | Index | Project | Index |
| TiO 2Content % | ≥98 | The coarse grain subnumber/ | 3 |
| Relative density | 3.9 | Median size/um | 0.35 (light transmission |
| Tinting strength | 1350 | 0～0.5um/％ | 79 |
| Oil number/g100g | 20～22 | 0.5～0.5um/％ | 15 |
| Screenings (325 order)/% | ≤0.02 | 0～1.0um/％ | 3 |
| Moisture/% | ≤0.3 | 1.0～1.5um/％ | 2 |
| The pH value | 7.0 | 1.5～2.0um/％ | 1 |
| Water dispersible/% | 93～96 | Resistance to chalking | Low |
The key technical indexes is:
| Project | Index | Project | Index | ||
| TiO2 content % | 98.3 | Oil number ,/g/100g≤ | 26 | ||
| Color (with the standard specimen ratio) | Be not less than | Screenings (325 order) % | ≤0.05 | ||
| The dry powder whiteness | Wg≥ | 95 | Water extract resistivity Ω m 〉= | 20 | |
| L≥ | 98.5 | Fe 2O 3Content, ppm≤ | 80 | ||
| a | -0.4～0.4 | The aqeous suspension pH value | 7.0～8.0 | ||
| b | -0.3～0.3 | Particle property | Median size um | ≤0.30 | |
| Reducing power (comparing 〉=) with standard specimen | 100 | 0.4um following % | ≥88.0 | ||
| 105 ℃ of volatile matter % (m/m) | 0.5 | 0.15um below | ≤15 | ||
| Through 23 ± 2 ℃ and relative humidity (50 ± 5) % pre-treatment 105 ℃ of volatile matter % of 24h (m/m) | ≤0.5 | The water solubles, % (m/m)≤ | 0.5 | ||
Embodiment
Realize that concrete steps of the present invention are as follows successively:
1, the F value of dense titanium liquid is controlled at: 1.9 ± 0.05, especially 1.9 ± 0.02
2, crystal seed dosage %:2.0 ± 0.5, especially 2.0 ± 0.2
Float back Fe when 3, washing
2O
3Content, ppm :≤50
4, salt is handled: through optimization Test, be adjusted into
P
2O
5%:0.18 ± 0.05, especially 0.18 ± 0.02
K
2O%:0.38 ± 0.05, especially 0.38 ± 0.02
5, kiln inlet amount control: 1.62 ± 0.04t/h
6, kiln temperature control:
Kiln hood: 960 ℃ ± 20 ℃
Kiln tail: 300 ℃ ± 10 ℃
7, kiln speed control system: 8 ± 2min/r
8, improvement of the present invention is, carried out optimization design, test and relevant important parameter has been carried out strict regulation control at the several important steps in the sulfuric acid method titanium pigment production process, and be combination standard to series of parameters.The F value of emphasizing dense titanium liquid at hydrolyzing process is controlled at: 1.9 ± 0.02.Suitably heighten the crystal seed dosage, other existing hydrolysising condition is constant, when so both having guaranteed pigment performance, and the metatitanic acid aggregate (TiO that hydrolysis generates
2.XSO
3.yH
2O) epigranular can be controlled at 0.8～1.1 micron, and what 0.4～2.0 micron distribution of metatitanic acid aggregate more in the past will be narrow is many.Be beneficial to the carrying out of filtering and washing simultaneously; Salt treatment agent dosage and brickkiln calcining temperature etc. are also stipulated within the specific limits, so just guaranteed that the whole process that the dehydration of calcining product, desulfurization and crystalline form are grown up in calcination process is comparatively steady.The product of burning till have characteristics such as color and luster is white, loose, reducing power height.Easily broken in the postorder crushing process, the granulometric facies of product are to concentrating, and branch is narrower, and coarse particles and fine particle are all less.Can satisfy 0.4um following 〉=88.0, the following % of 0.15um≤15 median size um≤0.30.Its pigment performance and particle property can satisfy the production demand of chemical fibre.Make titanium dioxide N Λ 300.
Embodiment (1):
1, titanium liquid F value 1.89
2, the crystal seed dosage 2.1%
3, back Fe content 30ppm is floated in washing
4, salt treatment agent dosage H
3PO
4(P
2O
5Meter) 0.2%
K
2CO
3(K
2The O meter) 0.38%
5, rotary kiln inlet amount 1.65t/h
6, Rotary Kiln Temperature control: 975 ± 5 ℃ of kiln hoods
300 ± 10 ℃ on kiln tail
7, kiln speed control system: 8 ' 30 "
8, comminution by gas stream
Embodiment
Embodiment (2):
1, titanium liquid F value 1.88
2, the crystal seed dosage 2.2%
3, back Fe content 25ppm is floated in washing
4, salt treatment agent dosage H
3PO
4(P
2O
5Meter) 0.2%
K
2CO
3(K
2The O meter) 0.38%
5, rotary kiln inlet amount 1.63t/h
6, Rotary Kiln Temperature control:
970 ± 5 ℃ of kiln hoods
300 ℃ on kiln tail
7, kiln speed control system: 8 ' 30 "
Claims (8)
1, the preparation method of anatase chemical fiber titanium dioxide, sulfuric acid process is carried out acidolysis, the leaching reduction, the titanium liquid after the sedimentation gets filtered liquid through after filtering, and the filtered liquid freezing and crystallizing is separated out FeSO
4, the filtrate adding auxiliary agent crystal seed that filtrate is refiltered the back gained is hydrolyzed, and separates out the metatitanic acid throw out in a large number and filters out the metatitanic acid solid; With the metatitanic acid is raw material, handles into the dense titanium liquid of titanyl sulfate of certain F value with the vitriol oil, handles precipitation with salt again, washes with water and drying, calcined by rotary kiln and pulverizing are prepared from, and the F value that it is characterized in that controlling dense titanium liquid is 1.9 ± 0.05; Add crystal seed 2.0 ± 0.5% in the hydrolytic process, its unit is a weight ratio of being converted into titanium dioxide.
2, by the described anatase chemical fiber titanium dioxide of claim 1 the preparation method, it is characterized in that adopting when salt is handled and add following element: P
2O
5%:0.18 ± 0.05, K
2O%:0.38 ± 0.05.
3, by claim 1 or 2 described anatase chemical fiber titanium dioxides the preparation method, the F value that it is characterized in that controlling dense titanium liquid is 1.9 ± 0.02.
4,, it is characterized in that adding following element: P by the preparation method of the described anatase chemical fiber titanium dioxide of claim 1
2O
5%: be 0.18 ± 0.02; K
2O%:0.38 ± 0.02.
5,, it is characterized in that crystal seed an amount of in the hydrolytic process 2.0 ± 0.2% by the preparation method of the described anatase chemical fiber titanium dioxide of claim 1.
6,, it is characterized in that kiln inlet amount control: 1.62 ± 0.04t/h by the preparation method of the described anatase chemical fiber titanium dioxide of claim 1.
7, by the described anatase chemical fiber titanium dioxide of claim 1 the preparation method, it is characterized in that kiln speed control system: 8 ± 2min/r.
8, by the described anatase chemical fiber titanium dioxide of claim 1 the preparation method, it is characterized in that the kiln temperature control condition of calcined by rotary kiln is: kiln hood: 960 ℃ ± 30 ℃, kiln tail: 300 ℃ ± 15 ℃.
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|---|---|---|---|
| CNB2006100402908A CN100355658C (en) | 2006-05-12 | 2006-05-12 | Method for preparing anatase chemical fiber special titanium pigment |
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| CN100355658C CN100355658C (en) | 2007-12-19 |
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Cited By (11)
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|---|---|---|---|---|
| CN101161353B (en) * | 2007-11-08 | 2010-06-02 | 周建国 | Method for obtaining titanium ore concentrate through floatation from titanium pigment acidolysis waste material by sulfate process |
| CN102153136A (en) * | 2011-02-25 | 2011-08-17 | 四川安宁铁钛股份有限公司 | Preparation method of hydrated titanium dioxide double-effect seed crystal |
| CN102219894A (en) * | 2010-04-15 | 2011-10-19 | 中国石油化工股份有限公司 | Method for producing semi-dulling titanium series polyester |
| CN102433034A (en) * | 2011-09-23 | 2012-05-02 | 江崴 | Novel technology for preparing pearlescent pigment |
| CN103657688A (en) * | 2012-09-12 | 2014-03-26 | 安徽迪诺环保新材料科技有限公司 | Tungsten-added type nanometre titanium dioxide catalyst for flue gas denitrification and preparation method for catalyst |
| CN103772672A (en) * | 2012-10-25 | 2014-05-07 | 中国石油化工股份有限公司 | Production method for full-dull titanium polyurethane |
| CN104058452A (en) * | 2013-12-05 | 2014-09-24 | 攀钢集团攀枝花钢铁研究院有限公司 | Settlement titanium liquid processing method |
| CN105502481A (en) * | 2014-09-26 | 2016-04-20 | 河南佰利联化学股份有限公司 | Preparation method for anatase titanium dioxide |
| CN106186055A (en) * | 2016-06-30 | 2016-12-07 | 广西金茂钛业有限公司 | A kind of preparation method producing hydrolysis crystal seed in titanium dioxide technique and the delustering agent titanium dioxide of the method manufacture |
| CN113582222A (en) * | 2021-08-09 | 2021-11-02 | 苏州市宏丰钛业有限公司 | Chemical fiber grade titanium dioxide preparation method and system based on ferrous sulfate serving as byproduct |
| CN115611307A (en) * | 2022-10-31 | 2023-01-17 | 徐州钛白化工有限责任公司 | Preparation method of anatase titanium dioxide special for chemical fibers |
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| JP4153066B2 (en) * | 1997-12-01 | 2008-09-17 | 石原産業株式会社 | Method for producing strongly cohesive titanium oxide |
| CN1242923C (en) * | 2004-02-13 | 2006-02-22 | 四川龙蟒集团有限责任公司 | Preparation process for titanium white of golden red stone type |
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| CN101161353B (en) * | 2007-11-08 | 2010-06-02 | 周建国 | Method for obtaining titanium ore concentrate through floatation from titanium pigment acidolysis waste material by sulfate process |
| CN102219894A (en) * | 2010-04-15 | 2011-10-19 | 中国石油化工股份有限公司 | Method for producing semi-dulling titanium series polyester |
| CN102219894B (en) * | 2010-04-15 | 2013-03-06 | 中国石油化工股份有限公司 | Method for producing semi-dulling titanium series polyester |
| CN102153136A (en) * | 2011-02-25 | 2011-08-17 | 四川安宁铁钛股份有限公司 | Preparation method of hydrated titanium dioxide double-effect seed crystal |
| CN102153136B (en) * | 2011-02-25 | 2013-05-15 | 四川安宁铁钛股份有限公司 | Preparation method of hydrated titanium dioxide double-effect seed crystal |
| CN102433034A (en) * | 2011-09-23 | 2012-05-02 | 江崴 | Novel technology for preparing pearlescent pigment |
| CN103657688A (en) * | 2012-09-12 | 2014-03-26 | 安徽迪诺环保新材料科技有限公司 | Tungsten-added type nanometre titanium dioxide catalyst for flue gas denitrification and preparation method for catalyst |
| CN103657688B (en) * | 2012-09-12 | 2015-09-23 | 安徽迪诺环保新材料科技有限公司 | A kind ofly add tungsten type nanometer titanium dioxide Catalysts and its preparation method for denitrating flue gas |
| CN103772672B (en) * | 2012-10-25 | 2016-01-13 | 中国石油化工股份有限公司 | The production method of full-dull titanium polyester |
| CN103772672A (en) * | 2012-10-25 | 2014-05-07 | 中国石油化工股份有限公司 | Production method for full-dull titanium polyurethane |
| CN104058452A (en) * | 2013-12-05 | 2014-09-24 | 攀钢集团攀枝花钢铁研究院有限公司 | Settlement titanium liquid processing method |
| CN104058452B (en) * | 2013-12-05 | 2015-11-18 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method processing sedimentation titanium liquid |
| CN105502481A (en) * | 2014-09-26 | 2016-04-20 | 河南佰利联化学股份有限公司 | Preparation method for anatase titanium dioxide |
| CN106186055A (en) * | 2016-06-30 | 2016-12-07 | 广西金茂钛业有限公司 | A kind of preparation method producing hydrolysis crystal seed in titanium dioxide technique and the delustering agent titanium dioxide of the method manufacture |
| CN113582222A (en) * | 2021-08-09 | 2021-11-02 | 苏州市宏丰钛业有限公司 | Chemical fiber grade titanium dioxide preparation method and system based on ferrous sulfate serving as byproduct |
| CN115611307A (en) * | 2022-10-31 | 2023-01-17 | 徐州钛白化工有限责任公司 | Preparation method of anatase titanium dioxide special for chemical fibers |
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Effective date of registration: 20170621 Address after: 221011 No. 99 Tian Yong Road, Xuzhou Industrial Park, Jiangsu, Xuzhou Patentee after: Xuzhou titanium dioxide Chemical Co Ltd Address before: 210012 Jiangsu city of Nanjing province outside of China No. 198 line Patentee before: Nanjing Titanium Dioxide Chemical Co., Ltd. |
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