CN103900941B - A kind of characterizing method of rutile phase titanium dioxide particles sintering degree - Google Patents
A kind of characterizing method of rutile phase titanium dioxide particles sintering degree Download PDFInfo
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- CN103900941B CN103900941B CN201410100194.2A CN201410100194A CN103900941B CN 103900941 B CN103900941 B CN 103900941B CN 201410100194 A CN201410100194 A CN 201410100194A CN 103900941 B CN103900941 B CN 103900941B
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Abstract
The invention discloses a kind of characterizing method of rutile phase titanium dioxide particles sintering degree, measure the specific area of rutile titanium dioxide sample, know particle sintering degree by analyzing measured specific area value, wherein, described specific area value is less, and titanium dioxide granule sintering is more serious; Described specific area value is larger, more slightly or not sintering of titanium dioxide granule sintering. The present invention detects the specific 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.
Description
Technical field
The invention belongs to the production technical field of sulfuric acid method titanium pigment, relate to the sign inspection of titanium dioxide granuleSurvey technology field, more particularly, relates to a kind of sign of rutile phase titanium dioxide particles sintering degreeMethod.
Background technology
The formal name used at school of titanium dioxide is titanium dioxide, in the technique of Production By Sulfuric Acid Process rutile type titanium white, forgesBurning refers to that hydrolysis metatitanic acid is converted into titanium dioxide after a series of removal of impurities operations such as washing, rinsing, filtrationThe process of particle, this process mainly comprises that metatitanic acid dehydration desulfurization, transformation of crystal and TiO 2 particles are longLarge etc., its chemical equation is suc as formula shown in (1).
Formula (1)
In calcination process, need to make calcining materials reach following requirement: (1) makes by dehydration, desulfurizationIt is neutral that material reaches, and make crystal formation obtain 100% conversion; (2) even particle size is neat, and faceIt is 0.2～0.3 μ m that material level titanium dioxide requires particle average grain diameter, and grain shape is similar to ball-type; (3) calcining is rawThe titanium dioxide becoming does not have lattice defect, and physicochemical properties are stable, and pigment performance is high.
In industrial production, the calcining of metatitanic acid is generally carried out in rotary kiln, in order to reach above-mentioned every wantingAsk, the maximum temperature in rotary kiln is conventionally up to more than 1000 DEG C, and so high temperature is as easy as rolling off a log causes twoTitan oxide particles sintering, causes that pigment performance declines, the poor and particle of whiteness is difficult for pulverizing more firmly etc. to lackFall into, normal production and product quality are caused to serious impact. Therefore, should reduce even and keep away aborningThe generation of non-sintered phenomenon.
In domestic and foreign literature and patent, all have nothing to do in rutile phase titanium dioxide particles sintering degree characterizing methodReport, 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 in solving the problems of the technologies described aboveOr multiple.
The object of the present invention is to provide a kind of quantitatively characterizing rutile phase titanium dioxide particles sintering degreeMethod.
To achieve these goals, the invention provides a kind of rutile phase titanium dioxide particles sintering degreeCharacterizing method, measure the specific area of rutile titanium dioxide sample, by analyzing measured ratioSurface area values is known particle sintering degree, and wherein, described specific area value is less, and titanium dioxide granule burnsTie more serious; Described specific 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, and the average grain diameter of titanium dioxide granule is0.2～0.3μm。
An embodiment of the characterizing method of rutile phase titanium dioxide particles sintering degree according to the present invention,The step of the specific area of described mensuration rutile titanium dioxide sample specifically comprises: by rutile-type twoTitanium oxide sample is put into the sample cell of specific surface area measuring instrument, then according to described specific surface area measuring instrumentSetting program carry out the mensuration of specific area value.
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,After being ground, described rutile titanium dioxide sample carries out again the mensuration of specific area.
An embodiment of the characterizing method of rutile titanium dioxide sintering degree according to the present invention, when thanSurface area values < 6.0m2When/g, titanium dioxide granule sintering is serious; As specific area value > 6.0m2When/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, reducing power TCS < 1700 of rutile titanium dioxide sample, brightDegree Jans < 94.4, blue phase SCX < 2.0; When titanium dioxide granule sintering is slightly or not when sintering, rutileThe reducing power TCS of type titanium dioxide sample > 1700, brightness Jans > 94.4, blue phase SCX > 2.0.
The present invention detects the specific surface that obtains rutile phase titanium dioxide particles by specific surface area measuring instrumentLong-pending, and obtain and characterizing particles sintering degree by analyzing the data that detect, method of the present invention sectionLearn reasonable, simple and practical, workable, be in industry first propose quantitative detection titanium dioxideThe method of grain sintering degree, can instruct production titanium dioxide preferably.
Detailed description of the invention
Hereinafter, in connection with exemplary embodiment to rutile phase titanium dioxide particles sintering of the present inventionThe characterizing method of degree is elaborated.
The characterizing method of rutile phase titanium dioxide particles sintering degree of the present invention is to utilize specific area to surveyThe specific area value of determining instrument detection titanium dioxide granule judges the sintering journey of titanium dioxide granule in this sampleDegree. What specifically, specific surface area measuring instrument was mainly measured is the summary table that testing sample unit mass hasArea, it comprises external surface area and internal surface area. In the time of titanium dioxide granule generation sintering, titanium dioxideParticle can be reunited together each other, and its internal surface area is less; And when not sintering or slight of titanium dioxide granuleWhen sintering, titanium dioxide granule is loose condition (of surface) distribution agglomeration does not occur or occurs less, table in itArea is large and cause total specific area larger. Prove through system test, due to measured titanium dioxideThe specific area of sample is concrete numerical value, and ensureing that titanium dioxide sample is rutile-type crystal formationUnder prerequisite, the size of measured specific area value just in time reflect titanium dioxide sample sintering degree andThe quality of its pigment performance, judged result has higher accuracy, for characterizing rutile titanium dioxideParticle sintering degree provides concrete quantizating index, and characterization result accurately and reliably.
Specifically, characterizing method according to the present invention comprises the following steps:
First measure the specific area of rutile titanium dioxide sample, then by analyzing measured ratio tableArea value is known particle sintering degree. Wherein, if specific area value is less, titanium dioxide granule sinteringMore serious; If specific area value is larger, more slightly or not sintering of titanium dioxide granule sintering. Work as dioxyWhen change titanium particle sintering is serious, a large amount of particle aggregations becomes larger granule, has significantly reduced specific surfaceLong-pending value; But when titanium dioxide granule sintering is slight or during without sintering, a large amount of particles is mainly dispersity,Specific area value when specific area value is now significantly higher than the serious state of sintering.
According to one embodiment of present invention, as specific area value < 6.0m2When/g, titanium dioxide granule burnsKnot is serious; As specific area value > 6.0m2When/g, slightly or not sintering of titanium dioxide granule sintering. Generally, in the time of rutile content >=97% in titanium dioxide, just think that this titanium dioxide is rutile-typeTitanium dioxide. According to the present invention, ensureing that titanium dioxide sample is under the prerequisite of rutile titanium dioxide,Also when rutile content >=97% in titanium dioxide sample and the specific area value of titanium dioxide sample>6.0m2When/g, the pigment performance of sample is better, slightly or not sintering of titanium dioxide granule sintering, otherwisePigment performance is poor, and titanium dioxide granule sintering is serious.
And, in the time that titanium dioxide granule sintering is serious, the reducing power of rutile titanium dioxide sampleTCS < 1700, brightness Jans < 94.4, blue phase SCX < 2.0; When titanium dioxide granule sintering slightly or does not burnWhen knot, the reducing power TCS of rutile titanium dioxide sample > 1700, brightness Jans > 94.4, Lan XiangSCX > 2.0. Therefore, can also verify according to than table by measuring the pigment performance of titanium dioxide sampleThe titanium dioxide granule sintering degree that area value is judged.
The rutile titanium dioxide sample that the present invention measures is mainly pigmentary titanium dioxide, and itsThe average grain diameter of middle titanium dioxide granule is 0.2～0.3 μ m. Because the performance of pigmentary titanium dioxide is wantedAsk higher, particle sintering degree is larger on the impact of its pigment performance, therefore for pigmentary titanium dioxideThe sign of particle sintering degree is particularly crucial and important.
The step of the specific area of said determination rutile titanium dioxide sample can be real as followsExecute, 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 cell of specific surface area measuring instrument;
3) then carry out the mensuration of specific 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. QuietThe measuring principle of state volumetric method and method of testing can according to GB, " gas absorption BET method be measured solidMatter specific area " (GB/T19587-2004) carry out, therefore not to repeat here.
And the quality of surveying timing controlled rutile titanium dioxide sample is 1～3g, if sample qualityVery little, can affect the precision of determination data; If sample quality is too many, detect consuming time longlyer, affect workMake efficiency.
Preferably, the mensuration of specific area will be carried out again after above-mentioned rutile titanium dioxide sample grinding.Usually, the particle in the titanium dioxide obtaining after metatitanic acid calcining very easily adsorbs, reunites together, butThis reunion is soft-agglomerated, is just waited as ground and absorption and the particle of reuniting can be separated by external force.Therefore,, before measuring the indices such as TiO 2 pigment performance, conventionally to first grind to inhaleEcho the particle of reunion separately, thereby ensure the accuracy of measurement result.
Utilize said method can be comparatively accurately and the burning of judgement rutile phase titanium dioxide particles that can be quantitativeKnot degree. 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, these four groups of dioxiesThe numbering of changing titanium 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 cell of specific surface area measuring instrument, according to the set journey of specific surface area measuring instrumentOrder, sample is after the process such as super-dry, mensuration, and obtaining its specific area value is 7.66m2/ g, sentencesDetermine the not sintering of particle in this sample, measure the pigment performance of this sample: reducing power TCS is simultaneously1720, 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 cell of specific surface area measuring instrument, according to the set journey of specific surface area measuring instrumentOrder, sample is after the process such as super-dry, mensuration, and obtaining its specific area value is 5.43m2/ g, sentencesParticle sintering in fixed this sample is serious, measures the pigment performance of this sample: reducing power TCS is simultaneously1655, 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 cell of specific surface area measuring instrument, according to the set journey of specific surface area measuring instrumentOrder, sample is after the process such as super-dry, mensuration, and obtaining its specific area value is 5.56m2/ g, sentencesParticle sintering in fixed this sample is serious, measures the pigment performance of this sample: reducing power TCS is simultaneously1625, 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 cell of specific surface area measuring instrument, according to the set journey of specific surface area measuring instrumentOrder, sample is after the process such as super-dry, mensuration, and obtaining its specific area value is 7.41m2/ g, sentencesParticle sintering in fixed this sample is slight, measures the pigment performance of this sample: reducing power TCS is simultaneously1760, 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 scientific and reasonable, simple and practical, workable etc. excellentPoint, has directive significance to actual production.
Although described rutile phase titanium dioxide particles of the present invention in conjunction with exemplary embodiment aboveThe characterizing method of sintering degree, but those of ordinary skill in the art should be clear, do not depart from right wantIn the situation of the spirit and scope of asking, can carry out various amendments to above-described embodiment.
Claims (6)
1. a characterizing method for rutile phase titanium dioxide particles sintering degree, is characterized in that, measuresThe specific area of rutile titanium dioxide sample, knows particle by analyzing measured specific area valueSintering degree,
Wherein, described specific area value is less, and titanium dioxide granule sintering is more serious; Described specific areaBe worth larger, more slightly or not sintering of titanium dioxide granule sintering,
Wherein, as specific area value < 6.0m2When/g, titanium dioxide granule sintering is serious; Work as specific areaValue > 6.0m2When/g, slightly or not sintering of titanium dioxide granule sintering,
Wherein, in the time that titanium dioxide granule sintering is serious, the reducing power of rutile titanium dioxide sampleTCS < 1700, brightness Jans < 94.4, blue phase SCX < 2.0; When titanium dioxide granule sintering slightly or does not burnWhen knot, the reducing power TCS of rutile titanium dioxide sample > 1700, brightness Jans > 94.4, Lan XiangSCX>2.0。
2. the characterizing method of rutile phase titanium dioxide particles sintering degree according to claim 1,It is characterized in that, described rutile titanium dioxide sample is pigmentary titanium dioxide, titanium dioxide granuleAverage grain diameter be 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 area of described mensuration rutile titanium dioxide sample specifically comprises:Rutile titanium dioxide sample is put into the sample cell of specific surface area measuring instrument, then according to described ratioThe setting program of surface area test instrument carries out the mensuration of specific area value.
4. the characterizing method of rutile phase titanium dioxide particles sintering degree according to claim 3,It is characterized in that, described specific surface area measuring instrument adopts static capacity method measuring principle to measure.
5. according to the sign side of the rutile phase titanium dioxide particles sintering degree described in claim 1 or 3Method, 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,It is characterized in that, after described rutile titanium dioxide sample is ground, carry out again the mensuration of specific area.
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| 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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| CN101293200A (en) * | 2008-05-30 | 2008-10-29 | 内蒙古大学 | Method for preparing dual-perovskite type methyl hydride combustion catalyst containing titanium |
| CN101711226A (en) * | 2007-01-15 | 2010-05-19 | 圣戈本陶瓷及塑料股份有限公司 | Ceramic particle material and preparation method thereof |
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| CN101293200A (en) * | 2008-05-30 | 2008-10-29 | 内蒙古大学 | Method for preparing dual-perovskite type methyl hydride combustion catalyst containing titanium |
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