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CN107036959A - Titanium dioxide method for quickly testing weathering resistance - Google Patents

Titanium dioxide method for quickly testing weathering resistance Download PDF

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CN107036959A
CN107036959A CN201710244004.8A CN201710244004A CN107036959A CN 107036959 A CN107036959 A CN 107036959A CN 201710244004 A CN201710244004 A CN 201710244004A CN 107036959 A CN107036959 A CN 107036959A
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titanium dioxide
sample
alcohol
weathering resistance
value
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吴小平
刘勇
吕波
王海波
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Pangang Group Research Institute Co Ltd
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    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N17/00Investigating resistance of materials to the weather, to corrosion, or to light
    • G01N17/004Investigating resistance of materials to the weather, to corrosion, or to light to light

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Abstract

本发明涉及钛白粉耐候性检测分析方法领域,尤其是一种钛白粉耐候性快速检测方法。本发明所要解决的技术问题是提供一种以醇与钛白粉的光化学反应为原理进行检测,能够实现钛白粉耐候性的快速准确检测的钛白粉耐候性快速检测方法,包括以下步骤:A、首先测定基准样品光照前后的色差ΔE;B、按照上述步骤a至步骤f的方式测定待测钛白样品的ΔE,获得试样的ΔE;C、计算得到样品光催化活性值。本发明创造性利用醇与钛白粉的光化学反应原理,实现了钛白粉耐候性的快速准确检测。不仅大大的缩短了检测所需时间,也有效提高了检测的准确度和检测结果的时效性,更适宜于各种需要进行快速准确的钛白粉耐候性检测的场合。The invention relates to the field of detection and analysis methods for the weather resistance of titanium dioxide, in particular to a rapid detection method for the weather resistance of titanium dioxide. The technical problem to be solved by the present invention is to provide a kind of detection method based on the photochemical reaction of alcohol and titanium dioxide, which can realize the fast and accurate detection of titanium dioxide weather resistance, comprising the following steps: A. Measure the color difference ΔE of the reference sample before and after illumination; B. Measure the ΔE of the titanium dioxide sample to be tested according to the above steps a to step f, and obtain the ΔE of the sample; C. Calculate the photocatalytic activity value of the sample. The present invention creatively utilizes the photochemical reaction principle of alcohol and titanium dioxide to realize rapid and accurate detection of the weather resistance of titanium dioxide. It not only greatly shortens the time required for testing, but also effectively improves the accuracy of testing and the timeliness of testing results, and is more suitable for various occasions that require fast and accurate weather resistance testing of titanium dioxide.

Description

钛白粉耐候性快速检测方法Rapid detection method for weather resistance of titanium dioxide

技术领域technical field

本发明涉及钛白粉耐候性检测分析方法领域,尤其是一种钛白粉耐候性快速检测方法。The invention relates to the field of detection and analysis methods for the weather resistance of titanium dioxide, in particular to a rapid detection method for the weather resistance of titanium dioxide.

背景技术Background technique

耐候性是钛白粉的重要性质之一,直接决定其使用领域和使用寿命。目前,检测钛白粉耐候性的方法主要包括天然曝晒试验、人工加速老化法等方法。自然曝晒一般需要数年之久,而人工加速老化也需耗时几个月。两种方法都比较耗时,检测费用高,不能及时反映试样的耐候性能,不能满足产品开发和生产的需要。而且这两种检测方法都需要将颜料制成漆膜,不能测定分散性较差的钛白初品的耐候性,具有一定的局限性。光催化方法能够实现对钛白粉耐候性的快速检测,但目前文献报道较少,且在测试准确性、便捷性方面还有待提高。中国专利CN 102998249 A公开了光催化降解罗丹明B检测钛白粉耐候性的方法,CN105651683 A公开了光催化降解有机染料检测钛白粉耐候性的方法。光催化降解有机染料的方法虽然能够较为快速的检测钛白粉耐候性,但是有机染料容易吸附于钛白粉表面,造成测试误差较大。Weather resistance is one of the important properties of titanium dioxide, which directly determines its application field and service life. At present, the methods for testing the weather resistance of titanium dioxide mainly include natural exposure test, artificial accelerated aging method and other methods. Natural exposure generally takes years, while artificial accelerated aging can also take months. Both methods are time-consuming and costly, and cannot reflect the weather resistance of the sample in time, and cannot meet the needs of product development and production. Moreover, both of these two detection methods require the pigment to be made into a paint film, and cannot measure the weather resistance of the primary titanium dioxide product with poor dispersibility, which has certain limitations. The photocatalytic method can realize the rapid detection of the weather resistance of titanium dioxide, but there are few reports in the literature, and the accuracy and convenience of the test still need to be improved. Chinese patent CN 102998249 A discloses a method for photocatalytically degrading rhodamine B to detect the weather resistance of titanium dioxide, and CN105651683 A discloses a method for photocatalytically degrading organic dyes to detect the weather resistance of titanium dioxide. Although the method of photocatalytic degradation of organic dyes can quickly detect the weather resistance of titanium dioxide, organic dyes are easily adsorbed on the surface of titanium dioxide, resulting in large test errors.

发明内容Contents of the invention

本发明所要解决的技术问题是提供一种以醇与钛白粉的光化学反应为原理进行检测,能够实现钛白粉耐候性的快速准确检测的钛白粉耐候性快速检测方法。The technical problem to be solved by the present invention is to provide a rapid detection method for the weather resistance of titanium dioxide based on the principle of photochemical reaction between alcohol and titanium dioxide, which can realize rapid and accurate detection of the weather resistance of titanium dioxide.

本发明解决其技术问题所采用的技术方案是:钛白粉耐候性快速检测方法,其特征在于,包括以下步骤:The technical scheme that the present invention adopts to solve its technical problem is: titanium dioxide weather resistance rapid detection method, it is characterized in that, comprises the following steps:

A、首先测定基准样品光照前后的色差ΔE如下:A. First measure the color difference ΔE of the reference sample before and after illumination as follows:

a、将钛白粉基准样品与醇混匀:取一定量的醇与基准样品,混合一定时间使二者混合均匀;a. Mix the reference sample of titanium dioxide with alcohol: take a certain amount of alcohol and the reference sample, and mix them for a certain period of time to make them evenly mixed;

b、制样:取少量步骤a中基准样品与醇的混合物置于载玻片上,放上盖玻片制成样品;b. Sample preparation: take a small amount of the mixture of the reference sample and alcohol in step a, place it on a glass slide, and put a cover glass to make a sample;

c、测试光照前试样的明度值L*、红绿色相值a*、黄蓝色相值b*:用色差仪测试步骤b得到的样品的L*、a*、b*值,平行测试求出平均值,记为L* 、a* 、b* c. Test the lightness value L * , red-green phase value a * , and yellow-blue phase value b * of the sample before illumination: the L * , a * , and b * values of the sample obtained in step b of the colorimeter test are calculated in parallel. The average value is recorded as L * qian , a * qian , b * qian ;

d、光照:将载玻片上的样品置于光源的光束中心并照射进行反应;d. Illumination: place the sample on the glass slide at the center of the beam of the light source and irradiate it for reaction;

e、测试光照后试样的明度值L*、红绿色相值a*、黄蓝色相值b*:用色差仪测试光照后得到的样品的L*、a*、b*值,平行测试求出平均值,记为L* 、a* 、b* e. Lightness value L * , red-green phase value a * , yellow-blue phase value b * of the sample after testing the light: use a colorimeter to test the L * , a * , b * value of the sample obtained after the light, parallel test to find The average value is recorded as L * hou , a * hou , b * hou ;

f、获得基准样品的ΔE:计算光照前后基准样品的颜色变化ΔE:ΔE=((L* -L* )2+(a* -a* )2+(b* -b* )2)1/2f. Obtain the ΔE of the reference sample: calculate the color change ΔE of the reference sample before and after illumination: ΔE=((L * front- L * back ) 2 +(a * front- a * back ) 2 +(b * front- b * After ) 2 ) 1/2 ;

B、按照上述步骤a至步骤f的方式测定待测钛白样品的ΔE,获得试样的ΔE;B. Measure the ΔE of the titanium dioxide sample to be tested according to the above steps a to step f, and obtain the ΔE of the sample;

C、计算得到样品光催化活性值:C. Calculate the photocatalytic activity value of the sample:

进一步的是,步骤a中的醇为丙醇、丁醇、戊醇、丙二醇、丙三醇、丁二醇、戊二醇中的一种或多种。Further, the alcohol in step a is one or more of propanol, butanol, pentanol, propylene glycol, glycerol, butylene glycol, and pentylene glycol.

进一步的是,步骤a中钛白粉基准样品的加入量为0.5-5g,醇的加入量为0.25-5g,混合时间为1-5min。Further, in step a, the addition amount of the titanium dioxide reference sample is 0.5-5g, the addition amount of alcohol is 0.25-5g, and the mixing time is 1-5min.

进一步的是,步骤b中所取的钛白粉与醇的混合物量为0.02-0.2g。Further, the amount of the mixture of titanium dioxide and alcohol taken in step b is 0.02-0.2g.

进一步的是,步骤b中样品形状为圆形。Further, the shape of the sample in step b is circular.

进一步的是,步骤c和步骤e中平行测试的次数为3-7次。Further, the number of parallel tests in step c and step e is 3-7 times.

进一步的是,步骤d中光源为氙灯或紫外灯,光照时间为5分钟至5小时。Further, in step d, the light source is a xenon lamp or an ultraviolet lamp, and the illumination time is 5 minutes to 5 hours.

进一步的是,步骤A中所使用的基准样品为性质稳定且混合均匀的钛白粉初品、成品、无机包膜前的初品或无机包膜后的样品。Further, the reference sample used in step A is a stable and uniformly mixed titanium dioxide primary product, finished product, primary product before inorganic coating or sample after inorganic coating.

进一步的是,步骤A中所使用的基准样品为硫酸法或氯化法金红石型钛白粉初品。Further, the reference sample used in step A is the primary product of rutile titanium dioxide produced by sulfuric acid process or chloride process.

本发明的有益效果是:就传统的钛白粉耐候性检测方法而言,主要包括天然曝晒试验、人工加速老化法等方法。自然曝晒一般需要数年之久,而人工加速老化也需耗时几个月。两种方法都比较耗时,检测费用高,不能及时反映试样的耐候性能,不能满足产品开发和生产的需要。而且这两种检测方法都需要将颜料制成漆膜,不能测定分散性较差的钛白初品的耐候性,具有一定的局限性。而本发明创造性利用醇与钛白粉的光化学反应原理,实现了钛白粉耐候性的快速准确检测。不仅大大的缩短了检测所需时间,也有效提高了检测的准确度和检测结果的时效性,更适宜于各种需要进行快速准确的钛白粉耐候性检测的场合。The beneficial effect of the present invention is: as far as the traditional titanium dioxide weather resistance detection method is concerned, it mainly includes methods such as natural exposure test, artificial accelerated aging method and the like. Natural exposure generally takes years, while artificial accelerated aging can also take months. Both methods are time-consuming and costly, and cannot reflect the weather resistance of the sample in time, and cannot meet the needs of product development and production. Moreover, both of these two detection methods require the pigment to be made into a paint film, and cannot measure the weather resistance of the primary titanium dioxide product with poor dispersibility, which has certain limitations. However, the present invention creatively utilizes the principle of photochemical reaction between alcohol and titanium dioxide to realize rapid and accurate detection of the weather resistance of titanium dioxide. It not only greatly shortens the time required for testing, but also effectively improves the accuracy of testing and the timeliness of testing results, and is more suitable for various occasions that require fast and accurate weather resistance testing of titanium dioxide.

具体实施方式detailed description

钛白粉耐候性快速检测方法,包括以下步骤:The rapid detection method of weather resistance of titanium dioxide comprises the following steps:

A、首先测定基准样品光照前后的色差ΔE如下:A. First measure the color difference ΔE of the reference sample before and after illumination as follows:

a、将钛白粉基准样品与醇混匀:取一定量的醇与基准样品,混合一定时间使二者混合均匀;a. Mix the reference sample of titanium dioxide with alcohol: take a certain amount of alcohol and the reference sample, and mix them for a certain period of time to make them evenly mixed;

b、制样:取少量步骤a中基准样品与醇的混合物置于载玻片上,放上盖玻片制成样品;b. Sample preparation: take a small amount of the mixture of the reference sample and alcohol in step a, place it on a glass slide, and put a cover glass to make a sample;

c、测试光照前试样的明度值L*、红绿色相值a*、黄蓝色相值b*:用色差仪测试步骤b得到的样品的L*、a*、b*值,平行测试求出平均值,记为L* 、a* 、b* c. Test the lightness value L * , red-green phase value a * , and yellow-blue phase value b * of the sample before illumination: the L * , a * , and b * values of the sample obtained in step b of the colorimeter test are calculated in parallel. The average value is recorded as L * qian , a * qian , b * qian ;

d、光照:将载玻片上的样品置于光源的光束中心并照射进行反应;d. Illumination: place the sample on the glass slide at the center of the beam of the light source and irradiate it for reaction;

e、测试光照后试样的明度值L*、红绿色相值a*、黄蓝色相值b*:用色差仪测试光照后得到的样品的L*、a*、b*值,平行测试求出平均值,记为L* 、a* 、b* e. Lightness value L * , red-green phase value a * , yellow-blue phase value b * of the sample after testing the light: use a colorimeter to test the L * , a * , b * value of the sample obtained after the light, parallel test to find The average value is recorded as L * hou , a * hou , b * hou ;

f、获得基准样品的ΔE:计算光照前后基准样品的颜色变化ΔE:ΔE=((L* -L* )2+(a* -a* )2+(b* -b* )2)1/2f. Obtain the ΔE of the reference sample: calculate the color change ΔE of the reference sample before and after illumination: ΔE=((L * front- L * back ) 2 +(a * front- a * back ) 2 +(b * front- b * After ) 2 ) 1/2 ;

B、按照上述步骤a至步骤f的方式测定待测钛白样品的ΔE,获得试样的ΔE;B. Measure the ΔE of the titanium dioxide sample to be tested according to the above steps a to step f, and obtain the ΔE of the sample;

C、计算得到样品光催化活性值:C. Calculate the photocatalytic activity value of the sample:

本发明上述检测方法中的参数所代表的意义是这样的:L*表示明度,即明度值L*;a*即红绿色相值,表示从洋红色至绿色的范围,简称红绿色相;b*表示从黄色至蓝色的范围,简称黄蓝色相。通过将各个参数量化比对,并得到试样的色差ΔE以及基准样品的ΔE,最终即可得到光催化活性值。本发明的亮点在于利用醇与钛白粉的光化学反应原理,缩短了检测的时间,也大大提高了检测的准确率,其整体的检测效果远优于传统的检测方法。The meaning represented by the parameters in the above-mentioned detection method of the present invention is such : L * represents lightness, i.e. lightness value L * ; * Indicates the range from yellow to blue, referred to as the yellow-blue phase. By quantifying and comparing each parameter, and obtaining the color difference ΔE of the sample and the ΔE of the reference sample, the photocatalytic activity value can finally be obtained. The highlight of the present invention is that the photochemical reaction principle of alcohol and titanium dioxide is used to shorten the detection time and greatly improve the detection accuracy, and its overall detection effect is far superior to the traditional detection method.

另外,本发明的方法还适用于广泛的醇类,其中,步骤a中的醇为丙醇、丁醇、戊醇、丙二醇、丙三醇、丁二醇、戊二醇中的一种或多种。进一步的,为了检测的精准,步骤a中钛白粉基准样品的加入量为0.5-5g,醇的加入量为0.25-5g,混合时间为1-5min;步骤b中所取的钛白粉与醇的混合物量为0.02-0.2g。在实际检测时,一般选择将步骤b中样品形状设计为圆形,便于观测。作为本发明中数据处理的关键步骤,一般的,步骤c和步骤e中平行测试的次数为3-7次为宜。In addition, the method of the present invention is also applicable to a wide range of alcohols, wherein the alcohol in step a is one or more of propanol, butanol, pentanol, propylene glycol, glycerol, butylene glycol, and pentylene glycol kind. Further, for the accuracy of detection, the addition amount of titanium dioxide reference sample in step a is 0.5-5g, the addition amount of alcohol is 0.25-5g, and the mixing time is 1-5min; the titanium dioxide taken in step b and alcohol The amount of the mixture is 0.02-0.2 g. In actual detection, it is generally chosen to design the shape of the sample in step b as a circle, which is convenient for observation. As a key step of data processing in the present invention, generally, the number of parallel tests in step c and step e is preferably 3-7 times.

对于光源而言,步骤d中光源优选为氙灯或紫外灯,光照时间为5分钟至5小时。For the light source, the light source in step d is preferably a xenon lamp or an ultraviolet lamp, and the illumination time is 5 minutes to 5 hours.

另外,对于步骤A中所使用的基准样品,优选为性质稳定且混合均匀的钛白粉初品、成品、无机包膜前的初品或无机包膜后的样品,进一步的,所使用的基准样品为硫酸法或氯化法金红石型钛白粉初品。In addition, for the reference sample used in step A, it is preferably a stable and uniformly mixed titanium dioxide primary product, finished product, primary product before inorganic coating or sample after inorganic coating. Further, the reference sample used It is the primary product of rutile titanium dioxide by sulfuric acid method or chloride method.

传统的钛白粉耐候性检测方法而言,主要包括天然曝晒试验、人工加速老化法等方法。自然曝晒一般需要数年之久,而人工加速老化也需耗时几个月。两种方法都比较耗时,检测费用高,不能及时反映试样的耐候性能,不能满足产品开发和生产的需要。而且这两种检测方法都需要将颜料制成漆膜,不能测定分散性较差的钛白初品的耐候性,具有一定的局限性。本发明创造性利用醇与钛白粉的光化学反应原理,实现了钛白粉耐候性的快速准确检测。不仅大大的缩短了检测所需时间,也有效提高了检测的准确度和检测结果的时效性。Traditional titanium dioxide weather resistance testing methods mainly include natural exposure test, artificial accelerated aging method and other methods. Natural exposure generally takes years, while artificial accelerated aging can also take months. Both methods are time-consuming and costly, and cannot reflect the weather resistance of the sample in time, and cannot meet the needs of product development and production. Moreover, both of these two detection methods require the pigment to be made into a paint film, and cannot measure the weather resistance of the primary titanium dioxide product with poor dispersibility, which has certain limitations. The present invention creatively utilizes the photochemical reaction principle of alcohol and titanium dioxide to realize rapid and accurate detection of the weather resistance of titanium dioxide. It not only greatly shortens the time required for detection, but also effectively improves the accuracy of detection and the timeliness of detection results.

Claims (9)

1. titanium dioxide method for quickly testing weathering resistance, it is characterised in that comprise the following steps:
Aberration Δ E before and after A, first measure authentic specimen illumination is as follows:
A, titanium dioxide authentic specimen and alcohol mixed:A certain amount of alcohol and authentic specimen are taken, mixing certain time mixes the two Uniformly;
B, sample preparation:Take the mixture of authentic specimen and alcohol in a small amount of step a to be placed on slide, put cover glass and sample is made;
The brightness value L of c, test light according to preceding sample*, red green mutually value a*, champac hue value b*:Obtained with color difference meter testing procedure b Sample L*、a*、b*Value, parallel testing obtains average value, is designated as L* Before、a* Before、b* Before
D, illumination:Sample on slide is placed in the beam center of light source and irradiated and is reacted;
The brightness value L of e, test light according to rear sample*, red green mutually value a*, champac hue value b*:After being shone with color difference meter test light The L of the sample arrived*、a*、b*Value, parallel testing obtains average value, is designated as L* Afterwards、a* Afterwards、b* Afterwards
F, the Δ E for obtaining authentic specimen:The color change Δ E of authentic specimen before and after calculating illumination:Δ E=((L* Before-L* Afterwards)2+ (a* Before-a* Afterwards)2+(b* Before-b* Afterwards)2)1/2
B, the Δ E for determining in the way of above-mentioned steps a to step f titanium white sample to be measured, obtain the Δ E of sample;
C, calculating obtain sample photocatalytic activity value:
2. titanium dioxide method for quickly testing weathering resistance as claimed in claim 1, it is characterised in that:Alcohol in step a is propyl alcohol, One or more in butanol, amylalcohol, propane diols, glycerine, butanediol, pentanediol.
3. titanium dioxide method for quickly testing weathering resistance as claimed in claim 1 or 2, it is characterised in that:Titanium dioxide base in step a The addition of quasi- sample is 0.5-5g, and the addition of alcohol is 0.25-5g, and incorporation time is 1-5min.
4. titanium dioxide method for quickly testing weathering resistance as claimed in claim 1, it is characterised in that:The titanium white taken in step b The mixing object amount of powder and alcohol is 0.02-0.2g.
5. titanium dioxide method for quickly testing weathering resistance as claimed in claim 4, it is characterised in that:Sample shape is in step b It is circular.
6. titanium dioxide method for quickly testing weathering resistance as claimed in claim 1, it is characterised in that:Step c is parallel with step e The number of times of test is 3-7 times.
7. titanium dioxide method for quickly testing weathering resistance as claimed in claim 1, it is characterised in that:Light source is xenon lamp in step d Or uviol lamp, light application time is 5 minutes to 5 hours.
8. titanium dioxide method for quickly testing weathering resistance as claimed in claim 1, it is characterised in that:Base used in step A Quasi- sample is the first product before the stable and well mixed titanium dioxide primary product of property, finished product, inorganic coating or the sample after inorganic coating Product.
9. titanium dioxide method for quickly testing weathering resistance as claimed in claim 1, it is characterised in that:Base used in step A Quasi- sample is sulfuric acid process or chloride process rutile type titanium dioxide primary product.
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Application publication date: 20170811