CN103900941A - Characterization method of sintering degree of rutile titanium dioxide particles - Google Patents
Characterization method of sintering degree of rutile titanium dioxide particles Download PDFInfo
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- CN103900941A CN103900941A CN201410100194.2A CN201410100194A CN103900941A CN 103900941 A CN103900941 A CN 103900941A CN 201410100194 A CN201410100194 A CN 201410100194A CN 103900941 A CN103900941 A CN 103900941A
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Abstract
The invention discloses a characterization method of the sintering degree of rutile titanium dioxide particles. The characterization method is to measur the specific area of a rutile titanium dioxide sample to obtain the particle sintering degree through analyzing the measured specific area value, if the specific area value is small, the particle sintering of titanium dioxide is severe; if the specific area value is large, the particle sintering of titanium dioxide is mild or none. According to the invention, the specific area value of the rutile titanium dioxide particles is measured and obtained through a specific area tester and the particle sintering degree is obtained and characterized through analyzing the measured data; the characterization method is scientific, reasonable, simple, practical and strong in operability; a method for quantitatively measure the particle sintering degree of titanium dioxide is provided initially in the industry and the production of titanium white powder can be relatively well guided.
Description
Technical field
The invention belongs to the production technical field of sulfuric acid method titanium pigment, relate to the sign detection technique field of titanium dioxide granule, more particularly, relate to a kind of characterizing method of rutile phase titanium dioxide particles sintering degree.
Background technology
The formal name used at school of titanium dioxide is titania, in the technique of Production By Sulfuric Acid Process rutile type titanium white, calcining refers to that hydrolysis metatitanic acid is converted into the process of titanium dioxide granule after a series of removal of impurities operations such as washing, rinsing, filtration, this process mainly comprises that metatitanic acid dehydration desulfurization, transformation of crystal and TiO 2 particles grow up etc., and its chemical equation is suc as formula shown in (1).
In calcination process, need to make calcining materials reach following requirement: (1) makes material reach neutral by dehydration, desulfurization, and makes crystal formation obtain 100% conversion; (2) even particle size is neat, and pigment-level titanium dioxide to require particle mean grain size be 0.2～0.3 μ m, particle shape is similar to ball-type; (3) titania that calcining generates does not have lattice imperfection, and physicochemical property are stable, and pigment performance is high.
In commercial production, the calcining of metatitanic acid is generally carried out in rotary kiln, in order to reach above-mentioned requirements, maximum temperature in rotary kiln is conventionally up to more than 1000 ℃, so high as easy as rolling off a log titanium dioxide granule sintering that causes of temperature, cause that pigment performance declines, the poor and particle of whiteness is difficult for the defects such as pulverizing more firmly, normal production and product quality are caused to serious impact.Therefore, should reduce aborning the generation of even avoiding sintering phenomenon.
In domestic and foreign literature and patent, all have nothing to do in the report of rutile phase titanium dioxide particles sintering degree characterizing method, therefore a kind of method that can characterize rutile phase titanium dioxide particles sintering degree urgently.
Summary of the invention
For deficiency of the prior art, the object of the invention is to one or more in solving the problems of the technologies described above.
The object of the present invention is to provide a kind of method of quantitatively characterizing rutile phase titanium dioxide particles sintering degree.
To achieve these goals, the invention provides a kind of characterizing method of rutile phase titanium dioxide particles sintering degree, measure the specific surface area of rutile titanium dioxide sample, know particle sintering degree by analyzing measured specific surface area value, wherein, described specific surface area value is less, and titanium dioxide granule sintering is more serious; Described specific surface area value is larger, more slightly or not sintering of titanium dioxide granule sintering.
An embodiment of the characterizing method of rutile phase titanium dioxide particles sintering degree according to the present invention, described rutile titanium dioxide sample is pigmentary titanium dioxide, the mean grain size of titanium dioxide granule is 0.2～0.3 μ m.
An embodiment of the characterizing method of rutile phase titanium dioxide particles sintering degree according to the present invention, the step of the specific surface area of described mensuration rutile titanium dioxide sample specifically comprises: rutile titanium dioxide sample is put into the sample hose of specific surface area measuring instrument, then carried out the mensuration of specific surface area value according to the setting program of described specific surface area measuring instrument.
An embodiment of the characterizing method of rutile phase titanium dioxide particles sintering degree according to the present invention, described specific surface area measuring instrument adopts static capacity method measuring principle to measure.
An embodiment of the characterizing method of rutile phase titanium dioxide particles sintering degree according to the present invention, the quality of described rutile titanium dioxide sample is 1～3g.
An embodiment of the characterizing method of rutile phase titanium dioxide particles sintering degree according to the present invention, will carry out the mensuration of specific surface area again after described rutile titanium dioxide sample grinding.
An embodiment of the characterizing method of rutile titanium dioxide sintering degree according to the present invention, as specific surface area value <6.0m
2when/g, titanium dioxide granule sintering is serious; As specific surface area value > 6.0m
2when/g, slightly or not sintering of titanium dioxide granule sintering.
An embodiment of the characterizing method of rutile titanium dioxide sintered particles degree according to the present invention, in the time that titanium dioxide granule sintering is serious, the reducing power TCS<1700 of rutile titanium dioxide sample, brightness Jans<94.4, blue phase SCX<2.0; When titanium dioxide granule sintering is slightly or not when sintering, reducing power TCS>1700, the brightness Jans>94.4 of rutile titanium dioxide sample, blue phase SCX>2.0.
The present invention detects the specific surface area that obtains rutile phase titanium dioxide particles by specific surface area measuring instrument, and obtain and characterizing particles sintering degree by analyzing the data that detect, methodological science of the present invention is reasonable, simple and practical, workable, for the method for quantitative detection titanium dioxide granule sintering degree proposing first in industry, can instruct preferably production titanium dioxide.
Embodiment
Hereinafter, in connection with exemplary embodiment, the characterizing method of rutile phase titanium dioxide particles sintering degree of the present invention is elaborated.
The characterizing method of rutile phase titanium dioxide particles sintering degree of the present invention is to utilize the specific surface area value of specific surface area measuring instrument detection titanium dioxide granule to judge the sintering degree of titanium dioxide granule in this sample.Specifically, what specific surface area measuring instrument was mainly measured is the total surface area that testing sample unit mass has, and it comprises external surface area and internal surface area.In the time of titanium dioxide granule generation sintering, titanium dioxide granule can be reunited together each other, and its internal surface area is less; And when titanium dioxide granule is not when sintering or slight sintering, titanium dioxide granule is loose condition (of surface) and distributes agglomeration occurs or occurs less, its internal surface area is large and cause total specific surface area larger.Prove through system test, because the specific surface area of measured titanium dioxide sample is concrete numerical value, and guaranteeing that titanium dioxide sample is under the prerequisite of rutile-type crystal formation, the size of measured specific surface area value just in time reflects the sintering degree of titanium dioxide sample and the quality of pigment performance thereof, judged result has higher accuracy, provide concrete quantizating index for characterizing rutile phase titanium dioxide particles sintering degree, characterization result accurately and reliably.
Specifically, characterizing method according to the present invention comprises the following steps:
First measure the specific surface area of rutile titanium dioxide sample, then know particle sintering degree by analyzing measured specific surface area value.Wherein, if specific surface area value is less, titanium dioxide granule sintering is more serious; If specific surface area value is larger, more slightly or not sintering of titanium dioxide granule sintering.In the time that titanium dioxide granule sintering is serious, a large amount of particle aggregations becomes larger granule, has significantly reduced specific surface area value; But when titanium dioxide granule sintering is slight or during without sintering, a large amount of particles is mainly disperse state, specific surface area value when specific surface area value is now significantly higher than the serious state of sintering.
According to one embodiment of present invention, as specific surface area value <6.0m
2when/g, titanium dioxide granule sintering is serious; As specific surface area value > 6.0m
2when/g, slightly or not sintering of titanium dioxide granule sintering.Generally speaking,, in the time of rutile content >=97% in titania, just think that this titania is rutile titanium dioxide.According to the present invention, guaranteeing that titanium dioxide sample is under the prerequisite of rutile titanium dioxide, also as rutile content>=97% in titanium dioxide sample and the specific surface area value >6.0m of titanium dioxide sample
2when/g, the pigment performance of sample is better, slightly or not sintering of titanium dioxide granule sintering, on the contrary pigment performance is poor, and titanium dioxide granule sintering is serious.
And, in the time that titanium dioxide granule sintering is serious, the reducing power TCS<1700 of rutile titanium dioxide sample, brightness Jans<94.4, blue phase SCX<2.0; When titanium dioxide granule sintering is slightly or not when sintering, reducing power TCS>1700, the brightness Jans>94.4 of rutile titanium dioxide sample, blue phase SCX>2.0.Therefore, can also verify the titanium dioxide granule sintering degree of judging according to specific surface area value by measuring the pigment performance of titanium dioxide sample.
The rutile titanium dioxide sample that the present invention measures is mainly pigmentary titanium dioxide, and wherein the mean grain size of titanium dioxide granule is 0.2～0.3 μ m.Because the performance requirement of pigmentary titanium dioxide is higher, particle sintering degree is larger on the impact of its pigment performance, therefore particularly crucial and important for the sign of the particle sintering degree of pigmentary titanium dioxide.
The step of the specific surface area of said determination rutile titanium dioxide sample can be implemented as follows, but the invention is not restricted to this:
1) open specific surface area measuring instrument;
2) rutile titanium dioxide sample is put into the sample hose of specific surface area measuring instrument;
3) then carry out the mensuration of specific surface area value according to the setting program of described specific surface area measuring instrument.
Wherein, the specific surface area measuring instrument using adopts static capacity method measuring principle to measure.The measuring principle of static capacity method and method of testing can (GB/T19587-2004) be carried out according to GB " gas absorption BET method is measured solid matter specific surface area ", and therefore not to repeat here.
And the quality of surveying timing controlled rutile titanium dioxide sample is 1～3g, if sample quality very little, can affect the precision of determination data; If sample quality is too many, detect consuming time longlyer, affect work efficiency.
Preferably, the mensuration of specific surface area will be carried out again after above-mentioned rutile titanium dioxide sample grinding.Usually, the particle in the titania obtaining after metatitanic acid calcining very easily adsorbs, reunites together, but this reunion is soft-agglomerated, and waiting as ground by external force just can be by the particle of absorption and reunion separately.Therefore, before measuring the indices such as TiO 2 pigment performance, conventionally to first grind that the particle of absorption and reunion is separated, thereby guarantee the accuracy of measurement result.
Utilize said method can be comparatively accurately and the sintering degree of judgement rutile phase titanium dioxide particles that can be quantitative.Below in conjunction with example, the invention will be further elaborated, and example is only for the present invention is described, and do not limit the invention.
In example 1-4, characterize four groups with characterizing method of the present invention and calcined first products, the numbering of these four groups of titanium dioxide sample is respectively 1#, 2#, 3#, 4#.
Example 1:
Weigh the 1# sample of 1.0g after grinding, open after specific surface area measuring instrument preheating 10min simultaneously, 1# sample is put into the sample hose of specific surface area measuring instrument, according to the blas of specific surface area measuring instrument, be sample after the process such as super-dry, mensuration, obtaining its specific surface area value is 7.66m
2/ g, judges the not sintering of particle in this sample, measures the pigment performance of this sample: reducing power TCS simultaneously and be 1720, brightness Jans is 94.6, blue phase SCX is 3.05, and rutile content is 97.2%.
Example 2:
Weigh the 2# sample of 2.1g after grinding, open after specific surface area measuring instrument preheating 10min simultaneously, 2# sample is put into the sample hose of specific surface area measuring instrument, according to the blas of specific surface area measuring instrument, be sample after the process such as super-dry, mensuration, obtaining its specific surface area value is 5.43m
2/ g, judges that the particle sintering in this sample is serious, measures the pigment performance of this sample: reducing power TCS simultaneously and be 1655, brightness Jans is 93.8, blue phase SCX is 1.21, and rutile content is 99.1%.
Example 3:
Weigh the 3# sample of 3.0g after grinding, open after specific surface area measuring instrument preheating 10min simultaneously, 3# sample is put into the sample hose of specific surface area measuring instrument, according to the blas of specific surface area measuring instrument, be sample after the process such as super-dry, mensuration, obtaining its specific surface area value is 5.56m
2/ g, judges that the particle sintering in this sample is serious, measures the pigment performance of this sample: reducing power TCS simultaneously and be 1625, brightness Jans is 93.9, blue phase SCX is 0.87, and rutile content is 98.4%.
Example 4:
Weigh the 4# sample of 1.4g after grinding, open after specific surface area measuring instrument preheating 10min simultaneously, 4# sample is put into the sample hose of specific surface area measuring instrument, according to the blas of specific surface area measuring instrument, be sample after the process such as super-dry, mensuration, obtaining its specific surface area value is 7.41m
2/ g, judges that the particle sintering in this sample is slight, measures the pigment performance of this sample: reducing power TCS simultaneously and be 1760, brightness Jans is 94.52, blue phase SCX is 2.42, and rutile content is 97.8%.
In sum, method of the present invention has the advantages such as scientific and reasonable, simple and practical, workable, and actual production is had to directive significance.
Although described the characterizing method of rutile phase titanium dioxide particles sintering degree of the present invention above in conjunction with exemplary embodiment, but those of ordinary skills should be clear, in the case of not departing from the spirit and scope of claim, can carry out various modifications to above-described embodiment.
Claims (8)
1. a characterizing method for rutile phase titanium dioxide particles sintering degree, is characterized in that, measures the specific surface area of rutile titanium dioxide sample, knows particle sintering degree by analyzing measured specific surface area value,
Wherein, described specific surface area value is less, and titanium dioxide granule sintering is more serious; Described specific surface area value is larger, more slightly or not sintering of titanium dioxide granule sintering.
2. the characterizing method of rutile phase titanium dioxide particles sintering degree according to claim 1, is characterized in that, described rutile titanium dioxide sample is pigmentary titanium dioxide, and the mean grain size of titanium dioxide granule is 0.2～0.3 μ m.
3. the characterizing method of rutile phase titanium dioxide particles sintering degree according to claim 1, it is characterized in that, the step of the specific surface area of described mensuration rutile titanium dioxide sample specifically comprises: rutile titanium dioxide sample is put into the sample hose of specific surface area measuring instrument, then carried out the mensuration of specific surface area value according to the setting program of described specific surface area measuring instrument.
4. the characterizing method of rutile phase titanium dioxide particles sintering degree according to claim 3, is characterized in that, described specific surface area measuring instrument adopts static capacity method measuring principle to measure.
5. according to the characterizing method of the rutile titanium dioxide sintering degree described in claim 1 or 3, it is characterized in that, the quality of described rutile titanium dioxide sample is 1～3g.
6. the characterizing method of rutile phase titanium dioxide particles sintering degree according to claim 1, is characterized in that, carries out the mensuration of specific surface area after described rutile titanium dioxide sample is ground again.
7. the characterizing method of rutile phase titanium dioxide particles sintering degree according to claim 1, is characterized in that, as specific surface area value <6.0m
2when/g, titanium dioxide granule sintering is serious; As specific surface area value > 6.0m
2when/g, slightly or not sintering of titanium dioxide granule sintering.
8. according to the characterizing method of the rutile phase titanium dioxide particles sintering degree described in claim 1 or 7, it is characterized in that, in the time that titanium dioxide granule sintering is serious, the reducing power TCS<1700 of rutile titanium dioxide sample, brightness Jans<94.4, blue phase SCX<2.0; When titanium dioxide granule sintering is slightly or not when sintering, reducing power TCS>1700, the brightness Jans>94.4 of rutile titanium dioxide sample, blue phase SCX>2.0.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106645262A (en) * | 2016-12-31 | 2017-05-10 | 攀枝花东方钛业有限公司 | Method for detecting sintering degree of primary calcined particles of rutile titanium dioxide |
| CN106768344A (en) * | 2016-11-23 | 2017-05-31 | 攀钢集团钛业有限责任公司 | Accurate detection titanium dioxide primary product pigment refers to calibration method |
| CN107490659A (en) * | 2017-09-25 | 2017-12-19 | 攀钢集团研究院有限公司 | A kind of characterizing method of hydrated titanium dioxide Calcine Strength |
| CN107976385A (en) * | 2017-11-13 | 2018-05-01 | 龙蟒佰利联集团股份有限公司 | A kind of rapid assay methods of titanium dioxide crystallite dimension |
| CN108821338A (en) * | 2018-07-11 | 2018-11-16 | 无锡睿龙新材料科技有限公司 | A kind of preparation of stable state titanium dioxide fine particles and surface modifying method |
| CN110631949A (en) * | 2019-10-25 | 2019-12-31 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for evaluating grinding performance of titanium dioxide primary product by sulfuric acid process |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106768344A (en) * | 2016-11-23 | 2017-05-31 | 攀钢集团钛业有限责任公司 | Accurate detection titanium dioxide primary product pigment refers to calibration method |
| CN106768344B (en) * | 2016-11-23 | 2018-09-18 | 攀钢集团钛业有限责任公司 | Accurate detection titanium dioxide primary product pigment refers to calibration method |
| CN106645262A (en) * | 2016-12-31 | 2017-05-10 | 攀枝花东方钛业有限公司 | Method for detecting sintering degree of primary calcined particles of rutile titanium dioxide |
| CN107490659A (en) * | 2017-09-25 | 2017-12-19 | 攀钢集团研究院有限公司 | A kind of characterizing method of hydrated titanium dioxide Calcine Strength |
| CN107976385A (en) * | 2017-11-13 | 2018-05-01 | 龙蟒佰利联集团股份有限公司 | A kind of rapid assay methods of titanium dioxide crystallite dimension |
| CN108821338A (en) * | 2018-07-11 | 2018-11-16 | 无锡睿龙新材料科技有限公司 | A kind of preparation of stable state titanium dioxide fine particles and surface modifying method |
| CN110631949A (en) * | 2019-10-25 | 2019-12-31 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for evaluating grinding performance of titanium dioxide primary product by sulfuric acid process |
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