CN106768344A - Accurate detection titanium dioxide primary product pigment refers to calibration method - Google Patents
Accurate detection titanium dioxide primary product pigment refers to calibration method Download PDFInfo
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- CN106768344A CN106768344A CN201611036996.7A CN201611036996A CN106768344A CN 106768344 A CN106768344 A CN 106768344A CN 201611036996 A CN201611036996 A CN 201611036996A CN 106768344 A CN106768344 A CN 106768344A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 243
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 111
- 239000000049 pigment Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000001514 detection method Methods 0.000 title claims abstract description 18
- 238000000227 grinding Methods 0.000 claims abstract description 69
- 239000000047 product Substances 0.000 claims abstract description 41
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000012043 crude product Substances 0.000 claims abstract description 16
- 239000002002 slurry Substances 0.000 claims description 54
- 239000011521 glass Substances 0.000 claims description 24
- 239000004570 mortar (masonry) Substances 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 8
- 238000003825 pressing Methods 0.000 claims description 8
- 239000003921 oil Substances 0.000 claims description 7
- 235000019198 oils Nutrition 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- 235000021388 linseed oil Nutrition 0.000 claims description 5
- 239000000944 linseed oil Substances 0.000 claims description 5
- 239000006229 carbon black Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims 1
- 238000003801 milling Methods 0.000 abstract description 9
- 239000002245 particle Substances 0.000 abstract description 7
- 238000005259 measurement Methods 0.000 abstract description 4
- 230000002349 favourable effect Effects 0.000 abstract description 3
- 230000006641 stabilisation Effects 0.000 abstract description 3
- 238000011105 stabilization Methods 0.000 abstract description 3
- 238000003556 assay Methods 0.000 abstract description 2
- 235000010215 titanium dioxide Nutrition 0.000 description 91
- 239000000203 mixture Substances 0.000 description 7
- 238000011017 operating method Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000001507 sample dispersion Methods 0.000 description 1
- 238000001429 visible spectrum Methods 0.000 description 1
- 235000014692 zinc oxide Nutrition 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
- G01J3/46—Measurement of colour; Colour measuring devices, e.g. colorimeters
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/02—Investigating particle size or size distribution
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/251—Colorimeters; Construction thereof
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
- G01N23/20025—Sample holders or supports therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
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- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Dispersion Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Spectrometry And Color Measurement (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention belongs to titanium dioxide performance detection field, and in particular to a kind of accurate detection titanium dioxide primary product pigment refers to calibration method.When determining the performance of titanium dioxide primary product pigment for prior art measurement result it is inaccurate, it is unstable the problems such as, the present invention provides a kind of accurate detection titanium dioxide primary product pigment and refers to calibration method, comprises the following steps：A, sample treatment：Titanium dioxide crude product is ground into granularity≤1.5mm, is transferred in agate beveller and is ground 20 30min, grinding rate is 220r/min；B, the titanium dioxide primary product pigment to gained in step a carry out rutile content, reducing power, brightness and dispersiveness and determine.The present invention is ground treatment, precise control milling time and rotating speed to titanium dioxide crude product by agate beveller so that titanium dioxide crude product pigment particle size is evenly, it is dispersed more preferable, with the use of specific assay method, make the measurement result of titanium dioxide crude product pigment more accurate, favorable reproducibility.The inventive method is simple to operate, testing result stabilization, suitably promotes the use of.
Description
Technical field
The invention belongs to titanium dioxide performance detection field, and in particular to a kind of accurate detection titanium dioxide primary product pigment index
Method.
Background technology
Titanium dioxide is a kind of most commonly used non-toxic inorganic Chinese white of current purposes, in ink, coating, plastics, papermaking
Occupy larger application market etc. industry.
Determine titanium dioxide quality refer mainly to indicate rutile content, reducing power, whiteness, brightness, dispersiveness etc., existing city
The quality of titanium dioxide is uneven on field, and can accurate, stabilization detection titanium dioxide face without a kind of general effective method
Material index, causes titanium dioxide testing result very big with actual deviation, influences the judge to titanium dioxide performance.
The content of the invention
The technical problem to be solved in the present invention is：Prior art determine titanium dioxide primary product pigment performance when measurement result not
Accurately, unstable the problems such as.
The present invention solve technical problem technical scheme be：A kind of side of accurate detection titanium dioxide primary product pigment index is provided
Method.The method is comprised the following steps：
A, sample treatment
Titanium dioxide crude product is ground into granularity≤1.5mm, is transferred in agate beveller and is ground 20-30min, grinding rate is
220r/min；
B, the titanium dioxide primary product pigment to gained in step a carry out rutile content, reducing power, brightness and dispersiveness and survey
It is fixed；
Rutile content is determined：
Measured using Y-4Q type X- diffractometers, the titanium dioxide after step a is ground is put into sample preparation ring, compress sample
Product, light source is made with Cu targets, is measured, and is determined voltage 4OKV, is determined electric current 45mA；
Reducing power is determined：
The titanium dioxide after step a grindings is weighed, the black slurry of equivalent is added, mixed on plain grinding instrument, ground uniform, ground
Grind after terminating sample distribution on colourless glass plates, its X/Y/Z value is surveyed on differential colorimeter；Described black slurry is essence
Linseed oil processed, refined caster oil, carbon black and the cotton-shaped silica of high-purity lightweight prepare by weight the ﹕ 0.5 of 7 ﹕, 2 ﹕ 0.6 and
Into；
Brightness measuring：
The titanium dioxide after step a grindings is weighed, colourless slurry is added, titanium dioxide is 3 with the weight ratio of colourless slurry:2.8,
Mix on plain grinding instrument, grind uniform, grind after terminating sample distribution on colourless glass plates, it is surveyed on differential colorimeter
X/Y/Z values；Described colourless slurry is to refine linseed oil, refined caster oil and the cotton-shaped silica of high-purity lightweight by weight
It is prepared from than the ﹕ 0.3 of 4 ﹕ 1；
Measuring brightness：
Be measured using whiteness instrument, by step a grind after titanium dioxide be put into sample-pressing device, be pressed into surfacing,
Texture-free, without fault, spotless sample board；
Color measuring in mortar：
The titanium dioxide after step a grindings is weighed, the black slurry of equivalent is added, mixed on plain grinding instrument, ground uniform, ground
Grind after terminating sample distribution on colourless glass plates, its X/Y/Z value is surveyed on differential colorimeter；
The measure of dispersiveness：
Remaining sample after brightness will be determined, colourless slurry will be added, ground, uniform white slurry be mixed into, by it
Put to deeper one end of black square graceful fineness gauge wedge shape double flute, flat sample is scraped along the shallow end of groove in 1-2S using scraper, from vertical
In the graceful fineness gauge of unilateral observation black square in the direction of flute length, the graceful fineness gauge plate face of black square remains 20-30 ° with the angle of sight line,
Place sample and answer≤10s to reading duration interval.
Wherein, during above-mentioned accurate detection titanium dioxide primary product pigment refers to calibration method, the agate beveller type described in step a
Number it is120X3 three-head grinding machines, power is >=380W.
Wherein, during above-mentioned accurate detection titanium dioxide primary product pigment refers to calibration method, the agate beveller list described in step a
Alms bowl treating capacity≤30g.
Beneficial effects of the present invention are：The present invention is mainly ground place by agate beveller to titanium dioxide crude product
Reason, precise control milling time and grinding rotating speed so that evenly, more preferably, cooperation makes dispersiveness titanium dioxide crude product pigment particle size
Specific assay method is used, makes the measurement result of titanium dioxide crude product pigment more accurate, favorable reproducibility.The inventive method operation letter
Single, testing result stabilization is suitably promoted the use of.
Specific embodiment
Refer to calibration method the invention provides a kind of accurate detection titanium dioxide primary product pigment, comprise the following steps：
A, sample treatment
Titanium dioxide crude product is ground into granularity≤1.5mm, is transferred in agate beveller and is ground 20-30min, grinding rate is
220r/min；
B, the titanium dioxide primary product pigment to gained in step a carry out rutile content, reducing power, brightness and dispersiveness and survey
It is fixed；
Rutile content is determined：
Measured using Y-4Q type X- diffractometers, the titanium dioxide after step a is ground is put into sample preparation ring, compress sample
Product, light source is made with Cu targets, is measured, and is determined voltage 4OKV, is determined electric current 45mA；
Reducing power is determined：
The titanium dioxide after step a grindings is weighed, the black slurry of equivalent is added, mixed on plain grinding instrument, ground uniform, ground
Grind after terminating sample distribution on colourless glass plates, its X/Y/Z value is surveyed on differential colorimeter；Described black slurry is essence
Linseed oil processed, refined caster oil, carbon black and the cotton-shaped silica of high-purity lightweight prepare by weight the ﹕ 0.5 of 7 ﹕, 2 ﹕ 0.6 and
Into；
Brightness measuring：
The titanium dioxide after step a grindings is weighed, colourless slurry is added, titanium dioxide is 3 with the weight ratio of colourless slurry:2.8,
Mix on plain grinding instrument, grind uniform, grind after terminating sample distribution on colourless glass plates, it is surveyed on differential colorimeter
X/Y/Z values；Described colourless slurry is to refine linseed oil, refined caster oil and the cotton-shaped silica of high-purity lightweight by weight
It is prepared from than the ﹕ 0.3 of 4 ﹕ 1；
Measuring brightness：
Be measured using whiteness instrument, by step a grind after titanium dioxide be put into sample-pressing device, be pressed into surfacing,
Texture-free, without fault, spotless sample board；
Color measuring in mortar：
The titanium dioxide after step a grindings is weighed, the black slurry of equivalent is added, mixed on plain grinding instrument, ground uniform, ground
Grind after terminating sample distribution on colourless glass plates, its X/Y/Z value is surveyed on differential colorimeter；
The measure of dispersiveness：
Remaining sample after brightness will be determined, colourless slurry will be added, ground, uniform white slurry be mixed into, by it
Put to deeper one end of black square graceful fineness gauge wedge shape double flute, flat sample is scraped along the shallow end of groove in 1-2S using scraper, from vertical
In the graceful fineness gauge of unilateral observation black square in the direction of flute length, the graceful fineness gauge plate face of black square remains 20-30 ° with the angle of sight line,
Place sample and answer≤10s to reading duration interval.
Wherein, during above-mentioned accurate detection titanium dioxide primary product pigment refers to calibration method, the agate beveller type described in step a
Number it is120X3 three-head grinding machines, power is >=380W.
Wherein, during above-mentioned accurate detection titanium dioxide primary product pigment refers to calibration method, the agate beveller list described in step a
Alms bowl treating capacity≤30g.
The present invention is ground treatment to sample using agate beveller, and agate beveller grinding rate is fast, grinds more equal
Even, grinding effect is more preferable.Rotating speed and milling time by controlling agate beveller of the invention, the sample after common regulation grinding
Granularity and uniformity.Grinding rate is 220r/min, and during milling time 20-30min, grinding effect is best, the sample after treatment
More accurate, the favorable reproducibility in rutile content, reducing power, brightness and dispersiveness survey timing results.
The reducing power of pigment depends primarily on degree of the granules of pigments to absorption and the scattering of light.Titanium dioxide is in visible spectrum
It is interior, absorb very small, therefore the reducing power of titanium dioxide depends primarily on its scattered power, and scattered power is relevant with particle size.
In the range of certain particle size, reducing power increases with the increase of the uniformity of the size and granularity of particle diameter, with the change of particle diameter it is big and
Reduce.The present invention adjusts the particle size range of titanium dioxide by adjusting grinding rate and milling time, and milling time is 20-30min
When, titanium dioxide reducing power is bigger.
Additionally, when milling time is 20-30min, the whiteness and dispersiveness of titanium dioxide are better.
Explanation is further explained to specific embodiment of the invention with reference to embodiment, but is not indicated that and will be protected
Scope is limited in scope described in embodiment.
Embodiment 1 detects titanium dioxide primary product pigment with the inventive method
Titanium dioxide primary product pigment is detected as follows, and operating procedure is as follows：
A, sample treatment
Titanium dioxide crude product is ground into granularity≤1.5mm, is transferred in agate beveller and is ground 20min, grinding rate is
220r/min；
B, the titanium dioxide primary product pigment to gained in step a carry out rutile content, reducing power, brightness and dispersiveness and survey
It is fixed；
Rutile content is determined：
Measured using Y-4Q type X- diffractometers, the titanium dioxide after step a is ground is put into sample preparation ring, compress sample
Product, light source is made with Cu targets, is measured, and is determined voltage 4OKV, is determined electric current 45mA；
Reducing power is determined：
The titanium dioxide after step a grindings is weighed, the black slurry of equivalent is added, mixed on plain grinding instrument, ground uniform, ground
Grind after terminating sample distribution on colourless glass plates, its X/Y/Z value is surveyed on differential colorimeter；
Brightness measuring：
The titanium dioxide after step a grindings is weighed, colourless slurry is added, titanium dioxide is 3 with the weight ratio of colourless slurry:2.8,
Mix on plain grinding instrument, grind uniform, grind after terminating sample distribution on colourless glass plates, it is surveyed on differential colorimeter
X/Y/Z values；
Measuring brightness：
Be measured using whiteness instrument, by step a grind after titanium dioxide be put into sample-pressing device, be pressed into surfacing,
Texture-free, without fault, spotless sample board；
Color measuring in mortar：
The titanium dioxide after step a grindings is weighed, the black slurry of equivalent is added, mixed on plain grinding instrument, ground uniform, ground
Grind after terminating sample distribution on colourless glass plates, its X/Y/Z value is surveyed on differential colorimeter；
The measure of dispersiveness：
Remaining sample after brightness will be determined, colourless slurry will be added, ground, uniform white slurry be mixed into, by it
Put to deeper one end of black square graceful fineness gauge wedge shape double flute, flat sample is scraped along the shallow end of groove in 1-2S using scraper, from vertical
In the graceful fineness gauge of unilateral observation black square in the direction of flute length, the graceful fineness gauge plate face of black square remains 20-30 ° with the angle of sight line,
Place sample and answer≤10s to reading duration interval.
Embodiment 2 detects titanium dioxide primary product pigment with the inventive method
Titanium dioxide primary product pigment is detected as follows, and operating procedure is as follows：
A, sample treatment
Titanium dioxide crude product is ground into granularity≤1.5mm, is transferred in agate beveller and is ground 25min, grinding rate is
220r/min；
B, the titanium dioxide primary product pigment to gained in step a carry out rutile content, reducing power, brightness and dispersiveness and survey
It is fixed；
Rutile content is determined：
Measured using Y-4Q type X- diffractometers, the titanium dioxide after step a is ground is put into sample preparation ring, compress sample
Product, light source is made with Cu targets, is measured, and is determined voltage 4OKV, is determined electric current 45mA；
Reducing power is determined：
The titanium dioxide after step a grindings is weighed, the black slurry of equivalent is added, mixed on plain grinding instrument, ground uniform, ground
Grind after terminating sample distribution on colourless glass plates, its X/Y/Z value is surveyed on differential colorimeter；
Brightness measuring：
The titanium dioxide after step a grindings is weighed, colourless slurry is added, titanium dioxide is 3 with the weight ratio of colourless slurry:2.8,
Mix on plain grinding instrument, grind uniform, grind after terminating sample distribution on colourless glass plates, it is surveyed on differential colorimeter
X/Y/Z values；
Measuring brightness：
Be measured using whiteness instrument, by step a grind after titanium dioxide be put into sample-pressing device, be pressed into surfacing,
Texture-free, without fault, spotless sample board；
Color measuring in mortar：
The titanium dioxide after step a grindings is weighed, the black slurry of equivalent is added, mixed on plain grinding instrument, ground uniform, ground
Grind after terminating sample distribution on colourless glass plates, its X/Y/Z value is surveyed on differential colorimeter；
The measure of dispersiveness：
Remaining sample after brightness will be determined, colourless slurry will be added, ground, uniform white slurry be mixed into, by it
Put to deeper one end of black square graceful fineness gauge wedge shape double flute, flat sample is scraped along the shallow end of groove in 1-2S using scraper, from vertical
In the graceful fineness gauge of unilateral observation black square in the direction of flute length, the graceful fineness gauge plate face of black square remains 20-30 ° with the angle of sight line,
Place sample and answer≤10s to reading duration interval.
Embodiment 3 detects titanium dioxide primary product pigment with the inventive method
Titanium dioxide primary product pigment is detected as follows, and operating procedure is as follows：
A, sample treatment
Titanium dioxide crude product is ground into granularity≤1.5mm, is transferred in agate beveller and is ground 30min, grinding rate is
220r/min；
B, the titanium dioxide primary product pigment to gained in step a carry out rutile content, reducing power, brightness and dispersiveness and survey
It is fixed；
Rutile content is determined：
Measured using Y-4Q type X- diffractometers, the titanium dioxide after step a is ground is put into sample preparation ring, compress sample
Product, light source is made with Cu targets, is measured, and is determined voltage 4OKV, is determined electric current 45mA；
Reducing power is determined：
The titanium dioxide after step a grindings is weighed, the black slurry of equivalent is added, mixed on plain grinding instrument, ground uniform, ground
Grind after terminating sample distribution on colourless glass plates, its X/Y/Z value is surveyed on differential colorimeter；
Brightness measuring：
The titanium dioxide after step a grindings is weighed, colourless slurry is added, titanium dioxide is 3 with the weight ratio of colourless slurry:2.8,
Mix on plain grinding instrument, grind uniform, grind after terminating sample distribution on colourless glass plates, it is surveyed on differential colorimeter
X/Y/Z values；
Measuring brightness：
Be measured using whiteness instrument, by step a grind after titanium dioxide be put into sample-pressing device, be pressed into surfacing,
Texture-free, without fault, spotless sample board；
Color measuring in mortar：
The titanium dioxide after step a grindings is weighed, the black slurry of equivalent is added, mixed on plain grinding instrument, ground uniform, ground
Grind after terminating sample distribution on colourless glass plates, its X/Y/Z value is surveyed on differential colorimeter；
The measure of dispersiveness：
Remaining sample after brightness will be determined, colourless slurry will be added, ground, uniform white slurry be mixed into, by it
Put to deeper one end of black square graceful fineness gauge wedge shape double flute, flat sample is scraped along the shallow end of groove in 1-2S using scraper, from vertical
In the graceful fineness gauge of unilateral observation black square in the direction of flute length, the graceful fineness gauge plate face of black square remains 20-30 ° with the angle of sight line,
Place sample and answer≤10s to reading duration interval.
Titanium dioxide primary product pigment is detected when the milling time of comparative example 1 is different
Titanium dioxide primary product pigment is detected as follows, and operating procedure is as follows：
A, sample treatment
Titanium dioxide crude product is ground into granularity≤1.5mm, is transferred in agate beveller and is ground 10min, grinding rate is
220r/min；
B, the titanium dioxide primary product pigment to gained in step a carry out rutile content, reducing power, brightness and dispersiveness and survey
It is fixed；
Rutile content is determined：
Measured using Y-4Q type X- diffractometers, the titanium dioxide after step a is ground is put into sample preparation ring, compress sample
Product, light source is made with Cu targets, is measured, and is determined voltage 4OKV, is determined electric current 45mA；
Reducing power is determined：
The titanium dioxide after step a grindings is weighed, the black slurry of equivalent is added, mixed on plain grinding instrument, ground uniform, ground
Grind after terminating sample distribution on colourless glass plates, its X/Y/Z value is surveyed on differential colorimeter；
Brightness measuring：
The titanium dioxide after step a grindings is weighed, colourless slurry is added, titanium dioxide is 3 with the weight ratio of colourless slurry:2.8,
Mix on plain grinding instrument, grind uniform, grind after terminating sample distribution on colourless glass plates, it is surveyed on differential colorimeter
X/Y/Z values；
Measuring brightness：
Be measured using whiteness instrument, by step a grind after titanium dioxide be put into sample-pressing device, be pressed into surfacing,
Texture-free, without fault, spotless sample board；
Color measuring in mortar：
The titanium dioxide after step a grindings is weighed, the black slurry of equivalent is added, mixed on plain grinding instrument, ground uniform, ground
Grind after terminating sample distribution on colourless glass plates, its X/Y/Z value is surveyed on differential colorimeter；
The measure of dispersiveness：
Remaining sample after brightness will be determined, colourless slurry will be added, ground, uniform white slurry be mixed into, by it
Put to deeper one end of black square graceful fineness gauge wedge shape double flute, flat sample is scraped along the shallow end of groove in 1-2S using scraper, from vertical
In the graceful fineness gauge of unilateral observation black square in the direction of flute length, the graceful fineness gauge plate face of black square remains 20-30 ° with the angle of sight line,
Place sample and answer≤10s to reading duration interval.
Titanium dioxide primary product pigment is detected when the milling time of comparative example 2 is different
Titanium dioxide primary product pigment is detected as follows, and operating procedure is as follows：
A, sample treatment
Titanium dioxide crude product is ground into granularity≤1.5mm, is transferred in agate beveller and is ground 15min, grinding rate is
220r/min；
B, the titanium dioxide primary product pigment to gained in step a carry out rutile content, reducing power, brightness and dispersiveness and survey
It is fixed；
Rutile content is determined：
Measured using Y-4Q type X- diffractometers, the titanium dioxide after step a is ground is put into sample preparation ring, compress sample
Product, light source is made with Cu targets, is measured, and is determined voltage 4OKV, is determined electric current 45mA；
Reducing power is determined：
The titanium dioxide after step a grindings is weighed, the black slurry of equivalent is added, mixed on plain grinding instrument, ground uniform, ground
Grind after terminating sample distribution on colourless glass plates, its X/Y/Z value is surveyed on differential colorimeter；
Brightness measuring：
The titanium dioxide after step a grindings is weighed, colourless slurry is added, titanium dioxide is 3 with the weight ratio of colourless slurry:2.8,
Mix on plain grinding instrument, grind uniform, grind after terminating sample distribution on colourless glass plates, it is surveyed on differential colorimeter
X/Y/Z values；
Measuring brightness：
Be measured using whiteness instrument, by step a grind after titanium dioxide be put into sample-pressing device, be pressed into surfacing,
Texture-free, without fault, spotless sample board；
Color measuring in mortar：
The titanium dioxide after step a grindings is weighed, the black slurry of equivalent is added, mixed on plain grinding instrument, ground uniform, ground
Grind after terminating sample distribution on colourless glass plates, its X/Y/Z value is surveyed on differential colorimeter；
The measure of dispersiveness：
Remaining sample after brightness will be determined, colourless slurry will be added, ground, uniform white slurry be mixed into, by it
Put to deeper one end of black square graceful fineness gauge wedge shape double flute, flat sample is scraped along the shallow end of groove in 1-2S using scraper, from vertical
In the graceful fineness gauge of unilateral observation black square in the direction of flute length, the graceful fineness gauge plate face of black square remains 20-30 ° with the angle of sight line,
Place sample and answer≤10s to reading duration interval.
The testing result of embodiment and comparative example is as shown in table 1 below.
The titanium white crude product pigment index that the distinct methods of table 1 are determined
From embodiment and comparative example, using technical scheme, rutile content is higher, whiteness value, TCS and
SCX values are higher, and sample dispersion is more preferable, using detection method of the invention so that pigment index is more preferable.
Claims (3)
1. accurate detection titanium dioxide primary product pigment refers to calibration method, it is characterised in that comprise the following steps：
A, sample treatment
Titanium dioxide crude product is ground into granularity≤1.5mm, is transferred in agate beveller and is ground 20-30min, grinding rate is
220r/min；
B, the titanium dioxide primary product pigment to gained in step a carry out rutile content, reducing power, brightness and dispersiveness and determine；
Rutile content is determined：
Measured using Y-4Q type X- diffractometers, the titanium dioxide after step a is ground is put into sample preparation ring, compress sample, with
Cu targets make light source, are measured, and determine voltage 4OKV, determine electric current 45mA；
Reducing power is determined：
The titanium dioxide after step a grindings is weighed, the black slurry of equivalent is added, mixed on plain grinding instrument, ground uniform, grinding knot
After beam sample distribution on colourless glass plates, its X/Y/Z value is surveyed on differential colorimeter；Described black slurry is refined Asia
Edestan oil, refined caster oil, carbon black and the cotton-shaped silica of high-purity lightweight are prepared from by weight the ﹕ 0.5 of 7 ﹕, 2 ﹕ 0.6；
Brightness measuring：
The titanium dioxide after step a grindings is weighed, colourless slurry is added, titanium dioxide is 3 with the weight ratio of colourless slurry:2.8, flat
Mixing, grinding are uniform on mill instrument, grind after terminating sample distribution on colourless glass plates, and its X/Y/ is surveyed on differential colorimeter
Z values；Described colourless slurry is refined linseed oil, refined caster oil and the cotton-shaped silica of high-purity lightweight by weight 4 ﹕
1 ﹕ 0.3 is prepared from；
Measuring brightness：
It is measured using whiteness instrument, the titanium dioxide after step a is ground is put into sample-pressing device, is pressed into surfacing, without line
Reason, without fault, spotless sample board；
Color measuring in mortar：
The titanium dioxide after step a grindings is weighed, the black slurry of equivalent is added, mixed on plain grinding instrument, ground uniform, grinding knot
After beam sample distribution on colourless glass plates, its X/Y/Z value is surveyed on differential colorimeter；
The measure of dispersiveness：
Remaining sample after brightness will be determined, colourless slurry will be added, ground, be mixed into uniform white slurry, put to
Deeper one end of the graceful fineness gauge wedge shape double flute of black square, scrapes flat sample, from perpendicular to groove in 1-2S using scraper along the shallow end of groove
The graceful fineness gauge of unilateral observation black square in direction long, the graceful fineness gauge plate face of black square remains 20-30 ° with the angle of sight line, places
Sample answers≤10s to reading duration interval.
2. accurate detection titanium dioxide primary product pigment according to claim 1 refers to calibration method, it is characterised in that：In step a
Described agate beveller model120X3 three-head grinding machines, power is >=380W.
3. accurate detection titanium dioxide primary product pigment according to claim 1 refers to calibration method, it is characterised in that：In step a
Described agate beveller list alms bowl treating capacity≤30g.
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| CN114167087A (en) * | 2021-12-02 | 2022-03-11 | 攀钢集团重庆钛业有限公司 | Method for rapidly measuring and calculating average particle size of titanium dioxide product |
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