CN109725077A - A kind of test method of titanium dioxide pigment photocatalysis characteristic - Google Patents
A kind of test method of titanium dioxide pigment photocatalysis characteristic Download PDFInfo
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- CN109725077A CN109725077A CN201811638756.3A CN201811638756A CN109725077A CN 109725077 A CN109725077 A CN 109725077A CN 201811638756 A CN201811638756 A CN 201811638756A CN 109725077 A CN109725077 A CN 109725077A
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- titanium dioxide
- dioxide pigment
- isopropanol
- pigment
- test method
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Abstract
The present invention relates to a kind of test methods of titanium dioxide pigment photocatalysis characteristic, comprising the following steps: the pretreatment of step 1, titanium dioxide pigment sample；Step 2 weighs test specimen after cooling, and aqueous isopropanol is added；Titanium dioxide pigment sample is put into ultraviolet ageing case by step 3, according to the light sensitivity of pigment, exposure；Step 4, the test specimen for crossing uv-exposure, are put into supercentrifuge and are separated, and extract supernatant；The supernatant of taking-up is put into gas chromatograph and carries out analysis test by step 5, according to isopropanol and acetone peak, determines the content of its isopropanol and acetone, and then determine titanium dioxide pigment photocatalysis characteristic.The present invention by titanium dioxide pigment under ultraviolet irradiation, oxonium ion can lose two electronics and become elemental oxygen, there is the nascent state elemental oxygen of photochemical reaction release very high activity can aoxidize any organic media contacted with titanium dioxide, it is caused gradually to degrade.
Description
Technical field
The invention belongs to the detection fields of inorganic pigment, in particular to the test side of titanium dioxide pigment photocatalysis characteristic
Method.
Background technique
Titanium dioxide pigment (Titanium Dioxide Pigment) is commonly called as titanium dioxide, is a kind of using extensive, performance
Outstanding white pigment, main application include the fields such as coating, plastics, papermaking.Presently commercially available titanium dioxide pigment in order to
The performances such as dispersibility, reducing power, covering power and the weatherability of titanium dioxide are improved to facilitate client to use, are typically necessary to it
Carry out the processing of surface cladding.The surface cladding processing of titanium dioxide pigment includes inorganic surface treatment and organic surface treatment.City
The inorganic surface treatment coating that product generally uses is sold as hydrated alumina, hydrated silica, hydrous zirconium oxide(HZO) and aluminum phosphate
One of or multiple combinations, organic surface treatment of use be generally trimethylolpropane, trimethylolethane and poly- silicon
One of oxygen alkane.Titanium dioxide pigment has photocatalytic activity, and under ultraviolet irradiation, oxonium ion can lose two electronics
And become elemental oxygen (or nascent oxygen), photochemical reaction release nascent state elemental oxygen have very high activity can aoxidize and
Any organic media of titanium dioxide contact, causes it gradually to degrade, can be with by inorganic surface treatment and organic surface treatment
The photocatalysis performance of titanium dioxide pigment is improved, but because of the difference of process of surface treatment and operation control process, titanium dioxide face
The photocatalysis performance of material has differences.
In detection method of the existing titanium dioxide pigment in relation to catalytic performance, such as GB/T 23987-2009 " colored paint and clear
The artificial weathering aging of lacquer coat, which exposes to the open air, is exposed to fluorescent UV and water ", titanium dioxide pigment is prepared into coating by this method,
By different application system preparation paint plates, the weatherability of titanium dioxide is evaluated by the variation of paint plate.This process compares survey
It is long to try the period；Characterized using acid extracting, that is, take it is a certain amount of by coating handle titanium dioxide, be added 96% it is dense
Sulfuric acid (TiO2: the weight ratio 1~10% of 96% concentrated sulfuric acid), after reacting 2~5h under the conditions of 175 DEG C, check titanium white in acid solution
The meltage of powder.When titanium dioxide meltage is less in acid solution, it is believed that the sample surfaces have formed the film of continuous uniform densification
Layer, the photocatalysis characteristic (weatherability) having had.But since the film layers such as aluminium oxide, zirconium oxide are soluble in acid, the evaluation method
Practical titanium white powder particles photocatalysis shielding characteristic cannot be embodied；Natural solarization weatherability is close to actual conditions, but experimental period mistake
It is long, and weather is not reproducible, and laboratory is made to have non-repeated.Therefore, in order to more directly and quickly test titanium dioxide face
The photocatalysis performance of material, spy have invented this test method.
It is dedicated for the non-plastic containing surface cladding processed material by the test to titanium dioxide pigment photocatalysis characteristic
Grade titanium dioxide pigment tests out photocatalysis performance by the method, more directly can quickly reflect process of surface treatment
Situation is conducive to the improvement production technology of titanium white production producer, helps speed up the high-weatherability product matter of titanium dioxide industry
Amount is promoted.Therefore, a kind of detection method meaning for directly, quickly and accurately testing titanium dioxide pigment photocatalysis performance is developed
It is great.
Summary of the invention
The present invention provides a kind of titanium dioxide pigment catalytic performance that obtains to make up the deficiency of existing test method
Test method.Test method of the invention, by the pretreatment of sample, the molten sample of sample, sample exposes to the open air, sample separates, sample color
Spectrum analysis and etc. test out the photocatalysis performance of titanium dioxide pigment.
The present invention is realized by following testing scheme:
A kind of test method of titanium dioxide pigment catalytic performance, includes the following steps:
The pretreatment of step 1, titanium dioxide pigment sample: titanium dioxide pigment is put into vacuum oven in certain temperature
It is dried under degree.
Step 2, the step 1 for weighing equal quality test specimen after cooling, aqueous isopropanol is added, and (additional amount is dioxy
3~5 times for changing titanium pigment quality, moisture content < 0.02%)；
The titanium dioxide pigment sample of step 2 is put into ultraviolet ageing case by step 3, according to the light sensitivity of pigment, keeps 1-
It exposes within 2 hours.
Step 4, by step 3 test specimen that uv-exposure is crossed, be put into supercentrifuge and separated, revolving speed
After 10000rpm, time 15min, the limpid supernatant of about 2ML is extracted.
The supernatant taken out in step 4 is put into gas chromatograph and carries out analysis test by step 5, according to isopropanol and
Acetone peak determines the content of its isopropanol and acetone to get the test method of titanium dioxide pigment photocatalysis characteristic.
The present invention more preferably testing scheme are as follows:
In step 1, sample drying and processing is to carry out in a vacuum drying oven.
In step 2, sample media selects isopropanol, and wherein aqueous isopropanol dosage is the 3~5 of titanium dioxide pigment quality
Times, and water content < 0.02% of isopropanol.
In step 3, according to the light sensitive characteristic of titanium dioxide pigment, the sample UV exposure time is 1~2h.
In step 4, uses supercentrifuge and sample solution is separated, revolving speed requires 10000rpm, time 15min.
In step 5, the supernatant of taking-up, which is put into gas chromatograph, carries out analysis test, according to isopropanol and acetone peak,
Determine the content of its isopropanol and acetone.
Through control titanium dioxide pigment under ultraviolet irradiation, oxonium ion can lose two electronics and become the present invention
The nascent state elemental oxygen of elemental oxygen (or nascent oxygen), photochemical reaction release can be aoxidized with very high activity and titanium dioxide
Any organic media of titanium contact, causes it gradually to degrade, and according to isopropanol and acetone peak, measures containing for isopropanol and acetone
Measure the test method to get titanium dioxide pigment photocatalysis characteristic.
The prominent advantage of the present invention is the method for most directly, quickly and accurately testing titanium dioxide pigment photocatalysis performance.
The high-weatherability product quality for helping speed up titanium dioxide industry simultaneously is promoted.
Specific embodiment
Below with reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and
It is not to limit.
Embodiment 1
The test method of titanium dioxide pigment photocatalysis characteristic, sequentially includes the following steps:
The pretreatment of step 1, titanium dioxide pigment sample (chloridising: sial coated prod): titanium dioxide pigment is put
Enter vacuum oven to be dried at 80 DEG C.
Step 2, the step 1 for weighing equal quality test specimen after cooling, aqueous isopropanol is added, and (additional amount is dioxy
4 times for changing titanium pigment quality, moisture content < 0.02%)；
The titanium dioxide pigment sample of step 2 is put into ultraviolet ageing case by step 3, according to the light sensitivity of pigment, keeps 1
Hour exposure.
Step 4, by step 3 test specimen that uv-exposure is crossed, be put into supercentrifuge and separated, revolving speed
After 10000rpm, time 15min, the limpid supernatant of about 2ML is extracted.
The supernatant taken out in step 4 is put into gas chromatograph and carries out analysis test by step 5, according to isopropanol and
Acetone peak determines the content of its isopropanol and acetone.
Embodiment 2
The pretreatment of step 1, titanium dioxide pigment sample (chloridising: sial coated prod): titanium dioxide pigment is put
Enter vacuum oven to be dried at 80 DEG C.
Step 2, the step 1 for weighing equal quality test specimen after cooling, aqueous isopropanol is added, and (additional amount is dioxy
4 times for changing titanium pigment quality, moisture content < 0.02%)；
The titanium dioxide pigment sample of step 2 is put into ultraviolet ageing case by step 3, according to the light sensitivity of pigment, keeps 2
Hour exposure.
Step 4, by step 3 test specimen that uv-exposure is crossed, be put into supercentrifuge and separated, revolving speed
After 10000rpm, time 15min, the limpid supernatant of about 2ML is extracted.
The supernatant taken out in step 4 is put into gas chromatograph and carries out analysis test by step 5, according to isopropanol and
Acetone peak determines the content of its isopropanol and acetone.
Embodiment 3
The pretreatment of step 1, titanium dioxide pigment sample (sulfuric acid process: sial coated prod): titanium dioxide pigment is put
Enter vacuum oven to be dried at 80 DEG C.
Step 2, the step 1 for weighing equal quality test specimen after cooling, aqueous isopropanol is added, and (additional amount is dioxy
4 times for changing titanium pigment quality, moisture content < 0.02%)；
The titanium dioxide pigment sample of step 2 is put into ultraviolet ageing case by step 3, according to the light sensitivity of pigment, keeps 1
Hour exposure.
Step 4, by step 3 test specimen that uv-exposure is crossed, be put into supercentrifuge and separated, revolving speed
After 10000rpm, time 15min, the limpid supernatant of about 2ML is extracted.
The supernatant taken out in step 4 is put into gas chromatograph and carries out analysis test by step 5, according to isopropanol and
Acetone peak determines the content of its isopropanol and acetone.
Embodiment 4
The pretreatment of step 1, titanium dioxide pigment sample (sulfuric acid process: sial coated prod): titanium dioxide pigment is put
Enter vacuum oven to be dried at 80 DEG C.
Step 2, the step 1 for weighing equal quality test specimen after cooling, aqueous isopropanol is added, and (additional amount is dioxy
4 times for changing titanium pigment quality, moisture content < 0.02%)；
The titanium dioxide pigment sample of step 2 is put into ultraviolet ageing case by step 3, according to the light sensitivity of pigment, keeps 1
Hour exposure.
Step 4, by step 3 test specimen that uv-exposure is crossed, be put into supercentrifuge and separated, revolving speed
After 10000rpm, time 15min, the limpid supernatant of about 2ML is extracted.
The supernatant taken out in step 4 is put into gas chromatograph and carries out analysis test by step 5, according to isopropanol and
Acetone peak determines the content of its isopropanol and acetone.
Embodiment 5
The pretreatment of step 1, titanium dioxide pigment sample (sulfuric acid process: sial coated prod): titanium dioxide pigment is put
Enter vacuum oven to be dried at 80 DEG C.
Step 2, the step 1 for weighing equal quality test specimen after cooling, aqueous isopropanol is added, and (additional amount is dioxy
4 times for changing titanium pigment quality, moisture content < 0.02%)；
The titanium dioxide pigment sample of step 2 is put into ultraviolet ageing case by step 3, according to the light sensitivity of pigment, keeps 2
Hour exposure.
Step 4, by step 3 test specimen that uv-exposure is crossed, be put into supercentrifuge and separated, revolving speed
After 10000rpm, time 15min, the limpid supernatant of about 2ML is extracted.
The supernatant taken out in step 4 is put into gas chromatograph and carries out analysis test by step 5, according to isopropanol and
Acetone peak determines the content of its isopropanol and acetone.
Embodiment 6
The pretreatment of step 1, titanium dioxide pigment sample (sulfuric acid process: sial coated prod): titanium dioxide pigment is put
Enter vacuum oven to be dried at 80 DEG C.
Step 2, the step 1 for weighing equal quality test specimen after cooling, aqueous isopropanol is added, and (additional amount is dioxy
4 times for changing titanium pigment quality, moisture content < 0.02%)；
The titanium dioxide pigment sample of step 2 is put into ultraviolet ageing case by step 3, according to the light sensitivity of pigment, keeps 2
Hour exposure.
Step 4, by step 3 test specimen that uv-exposure is crossed, be put into supercentrifuge and separated, revolving speed
After 10000rpm, time 15min, the limpid supernatant of about 2ML is extracted.
The supernatant taken out in step 4 is put into gas chromatograph and carries out analysis test by step 5, according to isopropanol and
Acetone peak determines the content of its isopropanol and acetone.
Embodiment 7
The pretreatment of step 1, titanium dioxide pigment sample (chloridising: zirconium aluminium coated prod): titanium dioxide pigment is put
Enter vacuum oven to be dried at 80 DEG C.
Step 2, the step 1 for weighing equal quality test specimen after cooling, aqueous isopropanol is added, and (additional amount is dioxy
4 times for changing titanium pigment quality, moisture content < 0.02%)；
The titanium dioxide pigment sample of step 2 is put into ultraviolet ageing case by step 3, according to the light sensitivity of pigment, keeps 1
Hour exposure.
Step 4, by step 3 test specimen that uv-exposure is crossed, be put into supercentrifuge and separated, revolving speed
After 10000rpm, time 15min, the limpid supernatant of about 2ML is extracted.
The supernatant taken out in step 4 is put into gas chromatograph and carries out analysis test by step 5, according to isopropanol and
Acetone peak determines the content of its isopropanol and acetone.
Embodiment 8
The pretreatment of step 1, titanium dioxide pigment sample (chloridising: zirconium aluminium coated prod): titanium dioxide pigment is put
Enter vacuum oven to be dried at 80 DEG C.
Step 2, the step 1 for weighing equal quality test specimen after cooling, aqueous isopropanol is added, and (additional amount is dioxy
4 times for changing titanium pigment quality, moisture content < 0.02%)；
The titanium dioxide pigment sample of step 2 is put into ultraviolet ageing case by step 3, according to the light sensitivity of pigment, keeps 2
Hour exposure.
Step 4, by step 3 test specimen that uv-exposure is crossed, be put into supercentrifuge and separated, revolving speed
After 10000rpm, time 15min, the limpid supernatant of about 2ML is extracted.
The supernatant taken out in step 4 is put into gas chromatograph and carries out analysis test by step 5, according to isopropanol and
Acetone peak determines the content of its isopropanol and acetone.
Embodiment 9
The pretreatment of step 1, titanium dioxide pigment sample (sulfuric acid process: zirconium aluminium coated prod): titanium dioxide pigment is put
Enter vacuum oven to be dried at 80 DEG C.
Step 2, the step 1 for weighing equal quality test specimen after cooling, aqueous isopropanol is added, and (additional amount is dioxy
4 times for changing titanium pigment quality, moisture content < 0.02%)；
The titanium dioxide pigment sample of step 2 is put into ultraviolet ageing case by step 3, according to the light sensitivity of pigment, keeps 1
Hour exposure.
Step 4, by step 3 test specimen that uv-exposure is crossed, be put into supercentrifuge and separated, revolving speed
After 10000rpm, time 15min, the limpid supernatant of about 2ML is extracted.
The supernatant taken out in step 4 is put into gas chromatograph and carries out analysis test by step 5, according to isopropanol and
Acetone peak determines the content of its isopropanol and acetone.
Embodiment 10
The pretreatment of step 1, titanium dioxide pigment sample (sulfuric acid process: zirconium aluminium coated prod): titanium dioxide pigment is put
Enter vacuum oven to be dried at 80 DEG C.
Step 2, the step 1 for weighing equal quality test specimen after cooling, aqueous isopropanol is added, and (additional amount is dioxy
4 times for changing titanium pigment quality, moisture content < 0.02%)；
The titanium dioxide pigment sample of step 2 is put into ultraviolet ageing case by step 3, according to the light sensitivity of pigment, keeps 2
Hour exposure.
Step 4, by step 3 test specimen that uv-exposure is crossed, be put into supercentrifuge and separated, revolving speed
After 10000rpm, time 15min, the limpid supernatant of about 2ML is extracted.
The supernatant taken out in step 4 is put into gas chromatograph and carries out analysis test by step 5, according to isopropanol and
Acetone peak determines the content of its isopropanol and acetone.
The comparison of table one embodiment and other test methods
In table, the test method of value of chromatism △ E*: being by titanium dioxide pigment in amino acrylic resin baking vanish system,
Under equal conditions painting, spray plate, drying, film thickness are 50 μm, then paint plate are put into ultraviolet accelerated ageing instrument, light source
(UVB313) it after exposing 240h to the open air, detects chromatic aberration value (△ E*), " paint and varnish applies reference standard GB/T 23987-2009
The artificial weathering aging of layer, which exposes to the open air, is exposed to fluorescent UV and water ".The technique being surface-treated due to titanium dioxide pigment
Condition is different, leads between product that there is differences.It can be seen from the table the detection method of acid-soluble ratio is not suitable for the cladding production of zirconium aluminium
The test of product.The measurement of content of acetone is consistent with the results change trend that ultraviolet ageing is tested, and is suitable for different type product
Test.The detection method is suitable for promoting and applying in titanium dioxide industry directly, quickly, accurately.
Claims (8)
1. a kind of test method of titanium dioxide pigment photocatalysis characteristic, which is characterized in that the titanium dioxide pigment photocatalysis
The sample pretreatment and its sample preparation before ultraviolet ageing of the test needs of characteristic.
2. the test method of titanium dioxide pigment photocatalysis characteristic according to claim 1, which is characterized in that this method is put into
Sample separation process after ultraviolet ageing case and its aging.
3. the test method of titanium dioxide pigment photocatalysis characteristic according to claim 1 or 2, which is characterized in that according to
Isopropanol and acetone peak, determine the content of its isopropanol and acetone, determine titanium dioxide pigment photocatalysis characteristic.
4. the test method of titanium dioxide pigment photocatalysis characteristic according to claim 3, which is characterized in that according to isopropyl
Pure and mild acetone peak determines the content of its isopropanol and acetone to get the test method of titanium dioxide pigment photocatalysis characteristic.
5. the test method of titanium dioxide pigment photocatalysis characteristic, which comprises the steps of:
The pretreatment of step 1, titanium dioxide pigment sample: titanium dioxide pigment is put into vacuum oven at a certain temperature
It is dried；
Aqueous isopropanol is added in step 2, the step 1 for weighing equal quality test specimen after cooling, the aqueous isopropanol
Additional amount is 3~5 times of titanium dioxide pigment quality, moisture content < 0.02% of the aqueous isopropanol；
The titanium dioxide pigment sample of step 2 is put into ultraviolet ageing case by step 3, and according to the light sensitivity of pigment, holding 1~2 is small
When expose；
Step 4, by step 3 test specimen that uv-exposure is crossed, be put into supercentrifuge and separated, revolving speed 10000rpm,
After time 15min, the limpid supernatant of about 2ML is extracted；
The supernatant taken out in step 4 is put into gas chromatograph and carries out analysis test by step 5, according to isopropanol and acetone
Peak determines the content of its isopropanol and acetone to get the test method of titanium dioxide pigment photocatalysis characteristic.
6. the test method of titanium dioxide pigment photocatalysis characteristic according to claim 5, which is characterized in that in step 1,
The drying box is vacuum oven.
7. the test method of titanium dioxide pigment photocatalysis characteristic according to claim 5, which is characterized in that in step 2,
The additional amount of the aqueous isopropanol is 3~5 times of titanium dioxide pigment quality, moisture content < 0.02% of the aqueous isopropanol.
8. the test method of titanium dioxide pigment photocatalysis characteristic according to claim 5, which is characterized in that in step 4,
The centrifuge be supercentrifuge, revolving speed 10000rpm, the time 15 minutes.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2598441A1 (en) * | 2010-07-26 | 2013-06-05 | Waters Technologies Corporation | Superficially porous materials comprising a substantially nonporous core having narrow particle size distribution; process for the preparation thereof; and use thereof for chromatographic separations |
| CN107398275A (en) * | 2017-06-20 | 2017-11-28 | 内蒙古大学 | A kind of copper catalyst and reaction process of volatile corrosion inhibitor film isopropanol acetone |
-
2018
- 2018-12-29 CN CN201811638756.3A patent/CN109725077A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2598441A1 (en) * | 2010-07-26 | 2013-06-05 | Waters Technologies Corporation | Superficially porous materials comprising a substantially nonporous core having narrow particle size distribution; process for the preparation thereof; and use thereof for chromatographic separations |
| CN107398275A (en) * | 2017-06-20 | 2017-11-28 | 内蒙古大学 | A kind of copper catalyst and reaction process of volatile corrosion inhibitor film isopropanol acetone |
Non-Patent Citations (3)
| Title |
|---|
| IRICK JR G: "Determination of the photocatalytic activities of titanium dioxides and other white pigments", 《JOURNAL OF APPLIED POLYMER SCIENCE》 * |
| VAN DRIEL, B. A. 等，: "A quick assessment of the photocatalytic activity of TiO2 pigments - From lab to conservation studio!", 《MICROCHEMICAL JOURNAL》 * |
| 李家其 等: "二氧化钛颜料表面包覆及光活性评价研究进展", 《化工进展》 * |
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