CN110687055A - Characterization method of whiteness of primary titanium chloride white product - Google Patents
Characterization method of whiteness of primary titanium chloride white product Download PDFInfo
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- CN110687055A CN110687055A CN201910968159.5A CN201910968159A CN110687055A CN 110687055 A CN110687055 A CN 110687055A CN 201910968159 A CN201910968159 A CN 201910968159A CN 110687055 A CN110687055 A CN 110687055A
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- sample
- funnel
- whiteness
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- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 title claims description 15
- 238000012512 characterization method Methods 0.000 title description 5
- 238000003825 pressing Methods 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 25
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000004327 boric acid Substances 0.000 claims abstract description 14
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000002360 preparation method Methods 0.000 claims abstract description 6
- 239000004033 plastic Substances 0.000 claims abstract description 5
- 229920003023 plastic Polymers 0.000 claims abstract description 5
- 238000010408 sweeping Methods 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims description 5
- 235000010215 titanium dioxide Nutrition 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 230000000007 visual effect Effects 0.000 abstract description 10
- 238000001514 detection method Methods 0.000 abstract description 8
- 239000004408 titanium dioxide Substances 0.000 abstract description 2
- NSYYPXSKPGPMBW-UHFFFAOYSA-N [O-2].[O-2].[Ti+4].Cl Chemical compound [O-2].[O-2].[Ti+4].Cl NSYYPXSKPGPMBW-UHFFFAOYSA-N 0.000 abstract 1
- 239000011521 glass Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 235000021388 linseed oil Nutrition 0.000 description 3
- 239000000944 linseed oil Substances 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 238000003892 spreading Methods 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 2
- 208000003464 asthenopia Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000003340 mental effect Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000036651 mood Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 235000019198 oils Nutrition 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 238000011179 visual inspection Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000012463 white pigment Substances 0.000 description 1
Classifications
-
- 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
-
- 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
- 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
Landscapes
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- General Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectrometry And Color Measurement (AREA)
Abstract
The invention relates to a method for characterizing the whiteness of a primary titanium dioxide chloride product, belonging to the field of titanium dioxide application performance detection. (1) The piston of the sample pressing machine is put down by about 2-5 cm, and the oiled paper sheet is put into the sinking piston surface to be flattened; (2) putting the clean funnel into a sample pressing machine and rotationally pressing the oilpaper sheet; (3) sleeving a funnel sleeve on a funnel, carefully adding a ground sample in the funnel, flattening, and carefully adding a proper amount of boric acid along the edge of the funnel; (4) taking down the sleeve, putting the plastic sample pressing block into the sleeve, pressing and rotating the sleeve, finally adding a little boric acid into the funnel to cover the sample, carefully taking out the funnel, and sweeping the boric acid around the sample preparation device into the funnel; (5) placing and fixing a pressing head, and starting a pressing machine to prepare a sample; (6) taking out the prepared sample wafer, and placing the sample wafer in an irradiation surface of a containing dish to be tested; (7) and (4) measuring the L, a and b values by using a CM-5 spectrocolorimeter, and calculating the Hunter whiteness. Compared with a visual method, the method has higher accuracy and reliability.
Description
Technical Field
The invention belongs to the field of titanium dioxide application performance detection, and particularly relates to a characterization method of primary titanium chloride white whiteness.
Background
Titanium white is a nontoxic inorganic white pigment with the most extensive application at present, and has a large application market in the industries of printing ink, coating, plastics, paper making and the like.
The whiteness index of the primary chlorinated titanium dioxide entering a factory needs to be detected, and the whiteness of the primary chlorinated titanium dioxide is mainly detected by a visual method at present. The whiteness evaluation by a visual method is simple and feasible, but cannot be represented by accurate data, which is obviously not ideal for controlling the whiteness index of the product, and in addition, the visual method cannot completely overcome the influence of subjective factors, such as reduced repeatability caused by eye fatigue or mental mood fluctuation. The defects can be overcome by adopting an instrument to measure the whiteness, and a unified detection method is not formed in the current stage of detecting the whiteness of the chlorinated primary dry powder.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for characterizing the whiteness of a primary titanium white chloride product, which comprises the following steps:
(1) the piston of the sample pressing machine is put down by about 2-5 cm, and the oiled paper sheet is put into the sinking piston surface to be flattened;
(2) putting the clean funnel into a sample pressing machine and rotationally pressing the oilpaper sheet;
(3) sleeving a funnel sleeve on a funnel, carefully adding a sample in the funnel, flattening, and carefully adding a proper amount of boric acid along the edge of the funnel;
(4) taking down the sleeve, putting the plastic sample pressing block into the sleeve, pressing and rotating the sleeve, finally adding a little boric acid into the funnel to cover the sample, carefully taking out the funnel, and sweeping the boric acid around the sample preparation device into the funnel;
(5) placing and fixing a pressing head, and starting a pressing machine to prepare a sample;
(6) taking out the prepared sample wafer, and placing the sample wafer in an irradiation surface of a containing dish to be tested;
(7) and (4) measuring the L, a and b values by using a CM-5 spectrocolorimeter, and calculating the Hunter whiteness.
The titanium chloride primary product is usually supplied by upstream customers, the particle size of the primary product needs to be controlled within 150-350nm, and if the particle size exceeds the controlled particle size range, the particle size of the primary product is unqualified.
After the grain size of the titanium chloride white primary product entering the factory is controlled, the titanium chloride white primary product does not need to be ground before testing, and the sample is directly prepared.
In order to better complete the sample preparation process, the invention preferably adopts a ZHY-401P sample pressing machine, wherein the automatic sample pressing machine is provided with a pressure sensor and an automatic hydraulic system and is precisely controlled by a Programmable Logic Controller (PLC). The automatic sample pressing machine accurately controls the sample pressing machine to operate according to a PLC program and signals transmitted by the pressure sensor, and displays the working state of the sample pressing machine at any time; after a sample pressing mode is selected on the PLC, the whole process of sample pressing, pressure maintaining and mold stripping can be automatically completed only by pressing a start key, and sample pressing of any person at any time can be guaranteed to be completely consistent.
Wherein the adding amount of the sample in the step (3) is 2-8 g, and the adding amount of the boric acid is 2-8 g.
And (5) starting the sample presser in the step (5), and keeping the pressure for 15-40 seconds when the pressure reaches 20 KN.
The invention has the beneficial effects that:
aiming at titanium chloride white primary product dry powder, the method adopts a CM-5 spectrocolorimeter to measure L, a and b values by controlling the pressure and the pressure maintaining time in the sample pressing process of a sample pressing machine, and calculates the Hunter whiteness, and the whiteness detection result has higher accuracy and reliability than a visual method; the invention adopts the instrument detection, and the judgment is carried out by obtaining the conclusion through the intuitive data, so that the method is simple to operate, the working efficiency is improved, the errors generated by human factors are reduced, and the reference value of the test result is higher than that of the visual detection method.
Detailed Description
The invention is further illustrated and described by the following examples and comparative examples.
Example 1
The method for testing the whiteness of the titanium chloride initial product comprises the following steps:
1. the piston of the sample pressing machine is put down by about 3 cm, and the oiled paper sheet is put into the sinking piston surface to be flattened;
2. putting the clean funnel into a sample pressing machine and rotationally pressing the oilpaper sheet;
3. the funnel was fitted with a funnel, 3 grams of the milled sample was carefully added to the funnel and flattened, and a total of about 3 grams of boric acid was carefully added along the funnel edge;
4. taking down the sleeve, putting the plastic sample pressing block into the sleeve, pressing and rotating the sleeve, finally adding a little boric acid into the funnel to cover the sample, carefully taking out the funnel, and sweeping the boric acid around the sample preparation device into the funnel;
5. placing and fixing a pressure head, starting a pressure sample machine to prepare a sample, keeping the pressure for 30 seconds when a pressure gauge reaches 20KN, and automatically closing a switch;
6. taking out the prepared sample wafer, carefully removing the oil paper on the surface of the sample wafer, purging the surface of the sample by an ear washing ball, and then placing the flat and clean surface of the sample in an irradiation surface of a container to be detected;
7. the L, a, b values were measured with a CM-5 spectrocolorimeter to calculate the Hunter whiteness, and 3 samples were pressed under the same conditions for each batch.
In this embodiment, 10 titanium chloride initial dry powders are selected for whiteness detection, and are designated as 1#, 2#, 3#, 4#, 5#, 6#, 7#, and 8 #: 9#, 10#, the test results are shown in table 1.
TABLE 1
Comparative example 1
In the comparative example, 10 titanium chloride primary dry powders used in the test of example 1 were used, and the whiteness of the titanium chloride primary was measured by the existing visual method, and the specific steps were as follows:
1. weighing 2g of sample and placing the sample on a lower glass plate cleaned by an automatic grinding machine;
2. extracting 0.8ml refined linseed oil by a needle tube, adding the refined linseed oil on a sample, and fully mixing the pigment and the refined linseed oil by a knife tip of a knife;
3. spreading the slurry into strips approximately 50mm wide, approximately midway from the edge to the center of the lower glass sheet, and wiping the mixture with the knives as much as possible onto the upper glass sheet of the mill;
4. closing the grinder plate, applying a force of about 4.5kg to grind, grinding for 50 revolutions each time for four times, collecting the pulp on the two plates together by using a knife after grinding for one time, spreading the pulp into strips with the width of 50mm, and smearing the knife on the upper plate;
5. after grinding is finished, taking the slurry from the plate for later use;
6. spreading the prepared sample and the slurry of the standard sample on a colorless glass plate in the same direction, preparing an opaque strip with the width of not less than 25mm and the side length of not less than 40mm by using a wet film preparation device, and observing the surface of the opaque strip immediately after coating under scattered sunlight or a standard light source (the included angle between the glass plate and the sight line is 45 degrees);
7. the whiteness of the sample is evaluated by the visual method according to the color phase of the sample, wherein the color phase is similar to, not lower than or slightly worse than that of the standard sample.
The results of whiteness measurement of example 1 and comparative example 1 were ranked in descending order from top to bottom, and the results are shown in table 2.
TABLE 2
As can be seen from Table 2, the whiteness detection result of the titanium chloride initial product by adopting the characterization method of the invention is basically consistent with the conventional visual judgment result, so that the feasibility of the characterization method of the invention is proved, but inconsistent rules can be generated due to individual judgment difference during visual inspection, and the samples with relatively close results can not be accurately judged and sequenced when being visually inspected. Therefore, the whiteness of the dry powder Hunter is measured by a CM-5 spectrocolorimeter, and the whiteness value of the chlorinated primary product is represented by the method, so that the method has higher accuracy and reliability compared with a visual method.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (4)
1. The method for characterizing the whiteness of the primary titanium white chloride product is characterized by comprising the following steps of:
(1) the piston of the sample pressing machine is put down by about 2-5 cm, and the oiled paper sheet is put into the sinking piston surface to be flattened;
(2) putting the clean funnel into a sample pressing machine and rotationally pressing the oilpaper sheet;
(3) sleeving a funnel sleeve on a funnel, carefully adding a sample in the funnel, flattening, and carefully adding a proper amount of boric acid along the edge of the funnel;
(4) taking down the sleeve, putting the plastic sample pressing block into the sleeve, pressing and rotating the sleeve, finally adding a little boric acid into the funnel to cover the sample, carefully taking out the funnel, and sweeping the boric acid around the sample preparation device into the funnel;
(5) placing and fixing a pressing head, and starting a pressing machine to prepare a sample;
(6) taking out the prepared sample wafer, and placing the sample wafer in an irradiation surface of a containing dish to be tested;
(7) and (4) measuring the L, a and b values by using a CM-5 spectrocolorimeter, and calculating the Hunter whiteness.
2. The method for characterizing the whiteness of the primary titanium chloride white according to claim 1, wherein the method comprises the following steps: the particle size of the sample in the step (3) is controlled to be 150-350 nm.
3. The method for characterizing the whiteness of the primary titanium chloride white according to claim 1, wherein the method comprises the following steps: the adding amount of the sample in the step (3) is 2-8 g, and the adding amount of the boric acid is 2-8 g.
4. The method for characterizing the whiteness of the primary titanium chloride white according to claim 1, wherein the method comprises the following steps: and (5) starting the sample presser, and keeping the pressure for 15-40 seconds when the pressure reaches 20 KN.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910968159.5A CN110687055A (en) | 2019-10-12 | 2019-10-12 | Characterization method of whiteness of primary titanium chloride white product |
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| CN201910968159.5A CN110687055A (en) | 2019-10-12 | 2019-10-12 | Characterization method of whiteness of primary titanium chloride white product |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109030335A (en) * | 2018-10-26 | 2018-12-18 | 攀钢集团重庆钛业有限公司 | Titanium dioxide primary product weatherability evaluation method |
-
2019
- 2019-10-12 CN CN201910968159.5A patent/CN110687055A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109030335A (en) * | 2018-10-26 | 2018-12-18 | 攀钢集团重庆钛业有限公司 | Titanium dioxide primary product weatherability evaluation method |
Non-Patent Citations (2)
| Title |
|---|
| 李亨: "《颜色应用分类疵点》", 31 January 2001 * |
| 沈超: "全自动荧光分析样品制样机的开放与研究", 《中国优秀博硕士学位论文全文数据库硕士工程科技I辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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