CN110286082A - A kind of titanium dioxide weatherability method for rapidly testing and application - Google Patents
A kind of titanium dioxide weatherability method for rapidly testing and application Download PDFInfo
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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
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- 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
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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
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- G01N1/38—Diluting, dispersing or mixing samples
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- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
- G01N17/004—Investigating resistance of materials to the weather, to corrosion, or to light to light
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- 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
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Abstract
The invention belongs to titanium dioxide technical field of performance test, disclose a kind of titanium dioxide weatherability method for rapidly testing and application, method includes: 1) to be uniformly mixed the material for preparing test sample, and material formula is by weight are as follows: 100 parts of Corvic, 5-10 parts of titanium dioxide, 3-10 parts of lead salt stabilizer, 2-8 parts of haloflex, 1-3 parts of plasticiser, 3-20 parts of precipitated calcium carbonate, 1-3 parts of ACR-401,0.1-1 parts of paraffin；2) print is processed as using the mixture that extruder obtains step 1)；3) print for obtaining step 2 is tailored into test sample, and tests its color value L0、a0、b0；4) in water by test sample sealing, isolation air is exposed to the sun 2-48h, tests its color value L1、a1、b1；5) color difference for front and back of being exposed to the sun is calculated
Description
Technical field
The invention belongs to titanium dioxide technical field of performance test, and in particular to a kind of titanium dioxide weatherability method for rapidly testing
And application.
Background technique
Titanium dioxide be one kind be widely used in the most important white pigment of the industries such as coating, plastics, papermaking, ink it
One, and weatherability is the critical nature for influencing titanium dioxide and using field and service life.Currently, titanium dioxide weatherability detection method
It mainly include the methods of natural solarization test, artificial accelerated aging method.As long as natural solarization generally requires the several years, and artificial acceleration
Aging also needs the time-consuming several months or more, cannot reflect the weather resistance of titanium dioxide in time, and testing cost is higher, is not able to satisfy product
The urgent needs of exploitation and production.
The rapid detection method of titanium dioxide weatherability mainly passes through the text that the method for photocatalysis aging is realized, but reported at present
It offers less, and there are problems that test accuracy, in terms of convenience.Chinese patent literature CN105651683A is dropped by photocatalysis
The method for solving organic dyestuff detection titanium dioxide weatherability, patent document CN102998249A disclose the inspection of photocatalytic degradation rhodamine
The method for surveying titanium dioxide weatherability.The photocatalysis method of rhodamine and similar degradation of organic dyes, though it is resistance to can reflect titanium dioxide
Hou Xing, but titanium dioxide surface can adsorb organic dyestuff, and titanium dioxide is also easy mutually absorption in organic dye solution, causes titanium
White powder cannot be uniform and stable dispersion in the solution, influence the weatherability test of titanium dioxide, data reliability is lower.
Summary of the invention
In view of the above-mentioned problems existing in the prior art, the object of the present invention is to provide a kind of titanium dioxide weatherabilities quickly to test
Titanium dioxide is adequately dispersed and is cured in plastic basis material, do not contacted with the external world by method and application, without adsorption phenomena, because
This can accomplish the repeatability of good dispersion and detection data, in addition lead salt is used for the detection of titanium dioxide weatherability, can be real
Quick, efficient, the accurate detection of existing titanium dioxide weatherability.
The present invention provides a kind of titanium dioxide weatherability method for rapidly testing, comprising the following steps:
1) material for preparing test sample is uniformly mixed, material formula is by weight are as follows: 100 parts of Corvic, titanium
5-10 parts of white powder, 3-10 parts of lead salt stabilizer, 2-8 parts of haloflex, 1-3 parts of plasticiser, 3-20 parts of precipitated calcium carbonate, ACR-
401 1-3 parts, 0.1-1 parts of paraffin；
2) print is processed as using the mixture that extruder obtains step 1)；
3) print for obtaining step 2 is tailored into test sample, and tests its color value L0、a0、b0；
4) in water by test sample sealing, isolation air is exposed to the sun 2-48h, tests its color value L1、a1、b1；
5) color difference for front and back of being exposed to the sun is calculated, judge the good of titanium dioxide weatherability
It is bad.
According to the present invention, conventional lead salt stabilizer can be used in the lead salt stabilizer and plasticiser etc., for example, described
Lead salt stabilizer can be selected from three alkali lead sulfates, dibasic lead phosphite, tribasic lead maleate, dibasic lead stearate or two alkali
Formula lead phthalate；The plasticiser can be DEHP, DOP, DBP etc..
Preferably, in step 1), material mixed method includes: to sequentially add the material in formula in high mixer, 800-
10-15min is mixed under 1500rpm revolving speed, is taken out and is stood 12 hours.
Preferably, in step 2, the temperature of extruder is set as 160-200 DEG C.
Preferably, in step 4), the water of sealing test print be by the rainwater of degassing process, tap water, desalted water or
Ultrapure water.
Preferably, in step 4), the method being exposed to the sun is heavy natural sunning, ultraviolet ageing case is exposed to the sun or xenon lamp aging case is exposed to the sun.
It is further preferred that heavy natural sunning is direct sunlight under conditions of temperature > 35 DEG C, humidity > 70%.This method pushes away
Recommend summer use.
It is further preferred that the condition that ultraviolet ageing case is exposed to the sun includes: 40-65 DEG C, 0.76-0.83W/m2.The method four
Ji Jun can be used.
It is further preferred that the condition that xenon lamp aging case is exposed to the sun includes: 40-65 DEG C, 0.51-1.1W/m2.The method four seasons
It can be used.
The technological parameter not being limited in the present invention selects the usual manner of this field to carry out, for example, the survey of color difference
The operation such as examination.
According to the present invention, above-mentioned titanium dioxide weatherability method for rapidly testing can be resistance in titanium dioxide finished product or titanium dioxide base-material
It is applied in the test of time property.
Compared with prior art, the invention has the following beneficial effects:
1, the present invention uses rigid plastics sample preparation, ensure that the good dispersibility of titanium dioxide, no absorption and agglomeration, it is ensured that
The repeatability of weatherability test, while weatherability being accelerated to test；The test method is simple, and quickly, accurately, minimum 2 hours are
Weatherability test result can be provided.
2, the detection architecture of the invention by the way that the lead salt stabilizer of certain content to be added to titanium dioxide, utilizes titanium dioxide
Photocatalysis induce the redox reaction of lead salt print ash caused to become, ash when detecting titanium dioxide becomes more obvious,
Become by lead salt ash and Ti3+Ash becomes the synergistic effect that two kinds of titanium dioxide photocatalysis induction ashes cash elephant, accelerates the resistance to of titanium dioxide
The test of time property, test speed are obviously accelerated, concrete principle are as follows: and the weatherability of titanium dioxide is the integrality of surface inorganic coating,
Titanium dioxide under w light can be by Ti4+Become Ti3+It, will if in the incomplete situation of inorganic coating, having the participation of Pb ion
Pb ion conversion is elementary lead, and the addition of such lead salt keeps colour variation more obvious, increases the discrimination of weather-proof sex differernce；Such as
Fruit inorganic coating is complete, Ti4+Become Ti3+During, it not will lead to the variation of lead salt, lead salt can in weatherability test process
Using the effect as indicator.
3, the present invention is guaranteed during the light-catalyzed reaction of titanium dioxide using the method for water seal isolation air, moisture
Ample supply, by the Ti in titanium dioxide4+Through Photoinduced Reduction at caesious Ti3+, make caesious Ti3+In no oxygen
Environment in, cannot timely be oxidized to colourless Ti4+, accumulated in print, print ash promoted to cash the acceleration hair of elephant
It is raw, accelerate weatherability test, according to the color value variation degree Δ E of test sample, can quickly, efficiently, accurately test out titanium
The weatherability of white powder, this method is applicable to titanium dioxide finished product and titanium dioxide base-material carries out weatherability test.
4, the method for the present invention is adopted by exposure in sunshine, the exposure of ultraviolet ageing case or xenon lamp aging case exposure in summer and autumn
It is exposed to the sun accelerated test with water seal sunlight, testing expense is low, and it is annual that weatherability test is carried out in ultraviolet or xenon lamp aging case
It can carry out, not limited by natural conditions.
Specific embodiment
Technical solution of the present invention is clearly and completely described below in conjunction with the embodiment of the present invention, it is clear that retouched
The embodiment stated is only a part of the embodiment of the present invention, instead of all the embodiments.
Embodiment 1-3 is for illustrating titanium dioxide weatherability method for rapidly testing and application of the invention.
Embodiment 1
1) material formula of test sample is prepared by weight are as follows: 100 parts of Corvic, 5 parts of titanium dioxide, lead salt is stablized
3 parts of agent (three alkali lead sulfates), 2 parts of haloflex, 1 part of plasticiser (DEHP), 3 parts of precipitated calcium carbonate, 1 part of ACR-401, stone
0.1 part of wax；Material in formula is sequentially added in high mixer in order, 15min is mixed under 1000rpm revolving speed, takes out and stands
12 hours；
2) mixture for obtaining step 1) is added in the feed bin of extruder, and the temperature of extruder is set in 180 DEG C, squeezes out sample
Piece；
3) print for obtaining step 2 is tailored into the test sample of 3.5cm × 8cm, and tests its color value L0、a0、b0；
4) test sample is put into sink (tap water of degassing process), completely cuts off air, is put into the place (summer of direct sunlight
Noon high temperature fair weather: temperature > 35 DEG C, humidity > 70%), it is exposed to the sun after 2h, tests its color value L1、a1、b1；
5) color difference for front and back of being exposed to the sun is calculated, color difference is bigger, and weatherability is poorer.
Tri- kinds of test b LR-688, Sample A and Sample B samples, different technologies personnel couple are distinguished using the above method
Above-mentioned sample is tested using same test method, and data are as shown in table 1.
Embodiment 2
1) material formula of test sample is prepared by weight are as follows: 100 parts of Corvic, 10 parts of titanium dioxide, lead salt is steady
Determine 10 parts of agent (tribasic lead maleate), 8 parts of haloflex, 3 parts of plasticiser (DOP), 20 parts of precipitated calcium carbonate, ACR-401
3 parts, 1 part of paraffin；Material in formula is sequentially added in high mixer in order, 12min is mixed under 1200rpm revolving speed, is taken out
Stand 12 hours.
2) mixture for obtaining step 1) is added in the feed bin of extruder, and the temperature of extruder is set in 160 DEG C, is squeezed
Print out；
3) print for obtaining step 2 is tailored into the test sample of 3.5cm × 10cm, and tests its color value L0、a0、b0；
4) (test condition: 60 DEG C, 0.78W/m is put into ultraviolet ageing case after test sample being completely cut off air with water-stop2)；Cruelly
After shining 2h, its color value L is tested1、a1、b1；
5) color difference for front and back of being exposed to the sun is calculated。
Tested respectively using the above method different aluminium contents titanium dioxide Binder sample Sample-1, Sample-2 and
The weatherability of Sample-3, aluminium content more high-weatherability is better as the result is shown, and specific data are as shown in table 2.
Embodiment 3
1) material formula of test sample is prepared by weight are as follows: 100 parts of Corvic, 8 parts of titanium dioxide, lead salt is stablized
8 parts of agent (dibasic lead phthalate), 5 parts of haloflex, 2 parts of plasticiser (DBP), 10 parts of precipitated calcium carbonate, ACR-401
2 parts, 0.5 part of paraffin；Material in formula is sequentially added in high mixer in order, 10min is mixed under 1500rpm revolving speed, takes
Stand 12 hours out.
2) mixture for obtaining step 1) is added in the feed bin of extruder, and the temperature of extruder is set in 190 DEG C, is squeezed
Print out；
3) print for obtaining step 2 is tailored into the test sample of 3.5cm × 10cm, and tests its color value L0、a0、b0；
4) (test condition: 45 DEG C, 0.51W/m is put into xenon lamp aging case after test sample being completely cut off air with water-stop2)；Cruelly
After shining 2h, its color value L is tested1、a1、b1；
5) color difference for front and back of being exposed to the sun is calculated。
Test titanium dioxide sample BLR-688, sample-a, sample-b, sample-c, sample-d and sample respectively using the above method
The weatherability of product-e, the results are shown in Table 3.
Comparative example 1
Same sample in embodiment 1 is exposed to the sun 6000 hours in xenon lamp aging case, carries out weatherability test, as a result such as table 1
It is shown.
Comparative example 2
Same sample in embodiment 2 is exposed to the sun 1000 hours in UV ageing oven, weatherability test is carried out, as a result such as 2 institute of table
Show.
Comparative example 3
Same sample in embodiment 3 is tested into (conventional xenon lamp 6000h) using conventional xenon lamp weatherability, the results are shown in Table 3.
Table 1
The data of table 1 show that quick aging weatherability of the invention is tested, the result trend and conventional xenon lamp weatherability measured
The trend of test result is consistent.
Table 2
As shown in Table 2, the trend for the test result that the result and UV aging measured using method for rapidly testing of the invention is measured
Unanimously.
Table 3
As shown in Table 3, the weatherability trend for the sample that method of the invention measures becomes with conventional xenon lamp weatherability test result
Gesture is consistent.
By the data of table 1-3 it is found that the method for the present invention quick, efficient, accurate can distinguish titanium dioxide finished product and titanium dioxide
The quality of base-material weatherability, can be as the substitution test method of conventional xenon lamp weatherability.
The embodiment of the present invention is described above, above description is exemplary, and non-exclusive, and also not
It is limited to disclosed embodiment.Without departing from the scope and spirit of illustrated embodiment, for the art
Many modifications and changes are obvious for those of ordinary skill.
Claims (10)
1. a kind of titanium dioxide weatherability method for rapidly testing, which comprises the following steps:
1) material for preparing test sample is uniformly mixed, material formula is by weight are as follows: 100 parts of Corvic, titanium
5-10 parts of white powder, 3-10 parts of lead salt stabilizer, 2-8 parts of haloflex, 1-3 parts of plasticiser, 3-20 parts of precipitated calcium carbonate, ACR-
401 1-3 parts, 0.1-1 parts of paraffin；
2) print is processed as using the mixture that extruder obtains step 1)；
3) print for obtaining step 2 is tailored into test sample, and tests its color value L0、a0、b0；
4) in water by test sample sealing, isolation air is exposed to the sun 2-48h, tests its color value L1、a1、b1；
5) color difference for front and back of being exposed to the sun is calculated, judge titanium dioxide weatherability
Quality.
2. titanium dioxide weatherability method for rapidly testing according to claim 1, it is characterised in that: the lead salt stabilizer choosing
From three alkali lead sulfates, dibasic lead phosphite, tribasic lead maleate, dibasic lead stearate or two alkali formula phthalic acids
Lead.
3. titanium dioxide weatherability method for rapidly testing according to claim 1, it is characterised in that: in step 1), material is mixed
Conjunction method includes: to sequentially add the material in formula in high mixer, and 10-15min is mixed under 800-1500rpm revolving speed, is taken out
Stand 12 hours.
4. titanium dioxide weatherability method for rapidly testing according to claim 1 or 3, it is characterised in that: in step 2, squeeze out
The temperature of machine is set as 160-200 DEG C.
5. titanium dioxide weatherability method for rapidly testing according to claim 1, it is characterised in that: in step 4), sealing is surveyed
The water of coupons is by the rainwater of degassing process, tap water, desalted water or ultrapure water.
6. titanium dioxide weatherability method for rapidly testing according to claim 1 or 5, it is characterised in that: in step 4), be exposed to the sun
Method be heavy natural sunning, ultraviolet ageing case is exposed to the sun or xenon lamp aging case is exposed to the sun.
7. titanium dioxide weatherability method for rapidly testing according to claim 6, it is characterised in that: heavy natural sunning is in temperature
> 35 DEG C, under conditions of humidity > 70%, direct sunlight.
8. titanium dioxide weatherability method for rapidly testing according to claim 6, it is characterised in that: ultraviolet ageing case is exposed to the sun
Condition includes: 40-65 DEG C, 0.76-0.83W/m2。
9. titanium dioxide weatherability method for rapidly testing according to claim 6, it is characterised in that: xenon lamp aging case is exposed to the sun
Condition includes: 40-65 DEG C, 0.51-1.1W/m2。
10. titanium dioxide weatherability method for rapidly testing described in any one of claim 1-9 is in titanium dioxide finished product or titanium white
Application in the test of powder base-material weatherability.
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| CN115420666A (en) * | 2022-09-29 | 2022-12-02 | 西南石油大学 | Positive freeze thawing soil gas permeability coefficient dynamic continuous testing system |
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| CN115420666A (en) * | 2022-09-29 | 2022-12-02 | 西南石油大学 | Positive freeze thawing soil gas permeability coefficient dynamic continuous testing system |
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| CN110286082B (en) | 2021-12-14 |
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