CN111307741B - Method for detecting hydrophobicity of color master batch-grade titanium dioxide - Google Patents
Method for detecting hydrophobicity of color master batch-grade titanium dioxide Download PDFInfo
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Abstract
The invention belongs to the technical field of chemical substance detection, and discloses a method for detecting hydrophobicity of color master-grade titanium dioxide, which comprises the following steps of mixing the color master-grade titanium dioxide with deionized water according to the mass-to-volume ratio of 1g:1L of the mixture is mixed and magnetically stirred, the stirring time is 0.5 to 1min, the stirring speed is 1000 to 1200r/min, and the mixed solution is kept stand for 10min after stirring to ensure that an oil film in the mixed solution is layered with turbid solution; and then, transferring a part of turbid liquid below the oil film into a measuring cylinder by using a transfer pipette, testing the absorbance of the turbid liquid by using a spectrophotometer within 1min, and comparing the test result with the absorbance of deionized water. The method can quickly detect the hydrophobicity of the color master-grade titanium dioxide and realize data quantification, and can represent the uniform degree of the coating of the organic coating agent on the titanium dioxide through the data quantification of the hydrophobicity, thereby being beneficial to quality evaluation and fine application of the color master-grade titanium dioxide.
Description
Technical Field
The invention belongs to the technical field of chemical substance detection, and particularly relates to a method for detecting hydrophobicity of color master batch-grade titanium dioxide.
Background
Titanium dioxide is the best white pigment in performance at present. It has acid and alkali resistance, whiteness, covering rate, high glossiness and weather resistance superior to other white pigments, and can be widely applied to the industrial fields of printing ink, coating, plastics, papermaking chemical fibers, cosmetics, rubber and the like. When the titanium white powder is applied to the fields of offset printing ink, plastics and the like, the hydrophobic property is also a very important index for measuring the quality of the titanium white powder. If the hydrophobicity is poor, the surface of the titanium dioxide is coated by polar groups (such as-0H), so that the titanium dioxide is easy to agglomerate due to polar adsorption or moisture absorption, when the titanium dioxide is used for plastic, the titanium dioxide is difficult to add, is easy to bond in a conveying pipeline, is easy to block a screen, and is difficult to uniformly disperse in a system during mixing even if the titanium dioxide is smoothly added into a mixing mill; when the titanium dioxide pigment is used for offset printing ink, the titanium dioxide pigment is required to have excellent hydrophobicity, because in the printing process of the offset printing ink, a resin binder must have good emulsification resistance so as to ensure that offset white ink cannot cause printing failure due to emulsification. Because offset printing completes the printing process according to the principle that oil and water repel, if titanium dioxide absorbs water, the printing is blurred, and the product cannot meet the use requirement.
The characterization method of the hydrophobicity of the titanium dioxide generally adopts a cold water floating method, namely, clear water is injected into a beaker, the water temperature is close to the room temperature, a proper amount of titanium dioxide is taken by a small spoon and is scattered on the water surface, the sedimentation condition is observed, and the slower the sedimentation is, the better the hydrophobicity is; on the contrary, the poorer the hydrophobicity, the longer the detection method is, the data quantization of the hydrophobicity of the titanium dioxide cannot be realized, and only the characterization effect can be achieved.
The adsorption modes of the organic coating agent and the titanium dioxide in the color master-grade titanium dioxide comprise a physical adsorption mode and a chemical adsorption mode, the existing titanium dioxide hydrophobicity characterization method is low in detection efficiency, the hydrophobicity of the color master-grade titanium dioxide cannot be subjected to data quantization, and the uniformity degree of the organic coating agent for coating the titanium dioxide cannot be characterized, so that the quality evaluation and the fine application of the color master-grade titanium dioxide are not facilitated.
Disclosure of Invention
In order to solve the technical problem, the invention provides a method for detecting hydrophobicity of color master batch-grade titanium dioxide, which comprises the following steps:
1) Mixing color master batch titanium dioxide and deionized water according to the mass to volume ratio of 1g: mixing the components in a proportion of 1L, magnetically stirring the components for 0.5 to 1min at a stirring speed of 1000 to 1200r/min, and standing the mixed solution for 10min after stirring to ensure that an oil film in the mixed solution is layered with turbid solution. When the stirring time is 0.5 to 1min, the repeatability of turbidity detection on the turbid liquid is better, and the stability detection on the absorbance of the turbid liquid is facilitated.
2) Transferring part of turbid liquid below the oil film into a measuring cylinder by using a transfer pipette, and testing the absorbance of the turbid liquid by using a spectrophotometer within 1 min; the detection is carried out within 1min, so that the influence of environmental factors on the test result can be reduced, a uniform detection standard is conveniently established, and the detection accuracy is improved.
3) Comparing the test result with the absorbance of the deionized water, wherein the closer the absorbance of the test result and the absorbance of the deionized water is, the better the hydrophobicity of the color master batch titanium dioxide is; conversely, the less hydrophobic. The better the hydrophobicity is, the higher the coating uniformity degree of the organic coating agent on the titanium dioxide is represented, so that the coating uniformity degree of the organic coating agent on the titanium dioxide in the color master-grade titanium dioxide is represented by the available absorbance, the data quantification of the rapid detection on the hydrophobicity of the color master-grade titanium dioxide is realized, and the quality evaluation and the fine application of the color master-grade titanium dioxide are facilitated.
Further, in the step 1), the weighing amount of the color master batch titanium dioxide is 1g, and the weighing amount of the deionized water is 1L, so that accurate metering and rapid stirring are facilitated.
Further, in the step 1), stirring the color master batch-grade titanium dioxide and deionized water in a 2L beaker, and placing a magnetic stirring rotor with the specification of C30 in the beaker. A2L beaker is matched with a magnetic stirring rotor with the specification of C30, so that the test result has better repeatability.
Further, in the step 1), the stirring time is 1min, the stirring speed is 1200r/min, and the shear force generated by stirring can separate the organic coating agent of the color master-grade titanium dioxide from the titanium dioxide to prepare the titanium dioxide mixed solution.
Further, in the step 2), 50 to 100ml of turbid liquid is put into a 100ml measuring cylinder, so that the absorbance of the turbid liquid can be conveniently detected.
Further, in step 3), the tuning wavelength of the spectrophotometer is 680nm.
In addition, the method can also be used for quickly judging the adsorption mode of the organic coating agent and the titanium dioxide in the color master-grade titanium dioxide, when the turbid liquid and the oil film are layered in the titanium dioxide mixed solution, the adsorption mode of the organic coating agent of the test sample is physical adsorption, and when the turbid liquid and the oil film are not layered, the deionized water below the beaker is kept clear, so that the adsorption mode of the organic coating of the color master-grade titanium dioxide is chemical adsorption.
The invention also comprises other conventional steps which can enable the color master batch grade titanium dioxide hydrophobicity detection method to be normally used, and all the conventional technical means in the field are adopted. In addition, the means or steps not limited in this invention are all the means of the conventional technology in this field.
In the invention, when the organic coating agent and the surface of the titanium dioxide are physically adsorbed, the organic coating agent and the titanium dioxide are separated by shear force generated during stirring by a magnetic stirrer, and the organic coating agent is gathered on the water surface due to hydrophobicity to form an oil film; and the titanium dioxide which is separated from the organic coating agent is dispersed in water because of the hydrophilicity, so that deionized water becomes turbid, if uncoated titanium dioxide exists, the titanium dioxide is dispersed in water without stirring to form turbid liquid, and a spectrophotometer is used for quickly detecting the absorbance of the turbid liquid within 1min, so that the data quantification of a test result is realized, and the uniform coating degree of the organic coating agent on the titanium dioxide in a sample is reflected. If the organic coating agent is chemically combined with the titanium dioxide, the organic coating agent and the titanium dioxide cannot be separated by stirring of a magnetic stirrer, so that the deionized water below is kept clear all the time, and no oil film is formed above the water surface.
The method has the advantages that the hydrophobicity of the color master-grade titanium dioxide can be rapidly detected, data quantization is realized, the uniform degree of the coating of the organic coating agent on the titanium dioxide can be represented by the data quantization of the hydrophobicity, and the quality evaluation and the fine application of the color master-grade titanium dioxide are facilitated.
Detailed Description
The present invention will be described more clearly with reference to specific embodiments thereof, which are given by way of illustration only and are not to be taken by way of limitation. All other embodiments, which can be obtained by those skilled in the art without any inventive step based on the embodiments of the present invention, should be included in the scope of the present invention.
Example 1
The invention provides a method for detecting hydrophobicity of color master batch-grade titanium dioxide, which comprises the following steps:
1) Weighing 1g of color master batch-grade titanium dioxide sample of LR-108 type by using weighing paper, weighing the soluble color master batch-grade titanium dioxide by using dimethyl silicone oil as an organic coating agent by using the weighing paper to ensure the metering accuracy, putting a magnetic stirring rotor of C30 specification into a beaker with the volume of 2L, measuring 1L of deionized water into the beaker by using a measuring cylinder, and adding the color master batch-grade titanium dioxide into the beaker; stirring the materials in the beaker by a magnetic stirrer, wherein the stirring time is 1min, the stirring speed is 1200r/min, the organic coating agent of the color master-grade titanium dioxide is separated from the titanium dioxide by the shearing force generated by stirring, and standing the beaker for 10min after stirring to ensure that an oil film in the mixed liquid in the beaker is layered with turbid liquid.
2) 50ml of turbid solution below the oil film is transferred into a 100ml measuring cylinder by a pipette, and the absorbance of the turbid solution is tested by a spectrophotometer within 1min, wherein the wavelength of the spectrophotometer is adjusted to 680nm, and the test results are 0.258, 0.263 and 0.253 respectively after 3 times of parallel experiments.
3) And comparing the test result with the absorbance of the deionized water (the detection value is 0.03), wherein the absorbance of the turbid liquid is close to the absorbance of the deionized water, which shows that the sample has good hydrophobicity and represents that the uniformity of the coating of the titanium dioxide by the organic coating agent is high.
Comparative example 1
The specification of the magnetic stirring rotor in example 1 was adjusted to C25, the other steps were not changed, and the absorbance test results of the turbid solution were: 0.083,0.032 and 0.063.
Comparative example 2
Taking 0.5g of color master batch grade titanium dioxide sample of LR-108 model by using weighing paper in example 1, measuring 0.5L of deionized water by using a measuring cylinder, selecting a beaker with the volume of 1L, carrying out parallel experiments for 3 times without changing other steps, wherein the absorbance test results of turbid liquid are respectively as follows: 0.138,0.150 and 0.166.
Comparative example 3
Taking 0.5g of color master batch grade titanium dioxide sample of LR-108 model by using weighing paper in example 1, measuring 0.5L of deionized water by using a measuring cylinder, adjusting the specification of a magnetic stirring rotor to be C25, selecting a beaker with the volume of 1L, carrying out parallel experiments for 3 times without changing other steps, wherein the absorbance test results of turbid liquid are respectively as follows: 0.079,0.042 and 0.068.
Comparing the examples with comparative examples 1 to 3, it can be seen from table 1 that the reproducibility of the test results is higher when a 2L beaker is used in combination with a magnetic stirring rotor of C30 specification.
Table 1: detection result of hydrophobicity (absorbance) of color master-grade titanium dioxide by different rotor and beaker sizes
Verification of sexual test
Five LR-108 color master batch grade titanium dioxide samples with known coating uniformity degrees of 100%, 99.5%, 99%, 98% and 95% are selected, and a verification test is respectively carried out by adopting the detection method of the invention, as can be seen from Table 2, the absorbance test results of the turbid liquid of each sample are respectively 0.045, 0.121, 0.596, 1.878 and 5.324, which shows that the discrimination of the invention on the hydrophobicity test of the titanium dioxide with different coating uniformity degrees is better, and meanwhile, the closer the absorbance of the turbid liquid is to the absorbance of deionized water (the detection value is 0.03), the better the hydrophobicity of the sample is, the higher the coating uniformity is, and conversely, the worse the hydrophobicity is, and the lower the coating uniformity is.
Table 2: test results of the validation test
In the above examples, comparative examples and verification tests, the organic coating agents of the selected samples are all in a physical adsorption mode, the organic coating agents are separated from titanium dioxide through shearing force generated during stirring by a magnetic stirrer, and the organic coating agents are gathered on the water surface due to hydrophobicity to form an oil film; and the titanium dioxide which is separated from the organic coating agent is dispersed in water because of the hydrophilicity of the titanium dioxide, so that deionized water becomes turbid, if uncoated titanium dioxide exists, the titanium dioxide is dispersed in water without stirring to form turbid liquid, and a spectrophotometer is used for quickly detecting the absorbance of the turbid liquid within 1min, so that the data quantification of a test result is realized, and the degree of uniform coating of the titanium dioxide by the organic coating agent in a sample is reflected.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the disclosed embodiments. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the illustrated embodiments.
Claims (6)
1. A color masterbatch level titanium dioxide hydrophobicity detection method is characterized by comprising the following steps:
1) Mixing color master batch titanium dioxide and deionized water according to the mass to volume ratio of 1g: mixing at a ratio of 1L, magnetically stirring for 0.5 to 1min at a stirring speed of 1000 to 1200r/min, and standing the mixed solution for 10min after stirring to layer an oil film in the mixed solution and a turbid solution;
2) Transferring part of turbid liquid below the oil film into a measuring cylinder by using a transfer pipette, and testing the absorbance of the turbid liquid by using a spectrophotometer within 1 min;
3) Comparing the test result with the absorbance of the deionized water, wherein the closer the absorbance of the test result and the absorbance of the deionized water is, the better the hydrophobicity of the color master batch titanium dioxide is; conversely, the less hydrophobic.
2. The method for detecting hydrophobicity of color masterbatch grade titanium dioxide according to claim 1, characterized in that: in the step 1), the weighing amount of the color master batch titanium dioxide is 1g, and the weighing amount of the deionized water is 1L.
3. The color master batch titanium dioxide hydrophobicity detection method according to claim 2, characterized in that: in the step 1), the color master batch-grade titanium dioxide and deionized water are stirred in a 2L beaker, and a magnetic stirring rotor with the specification of C30 is placed in the beaker.
4. The color masterbatch level titanium dioxide hydrophobicity detection method according to claim 3, characterized in that: in the step 1), the stirring time is 1min, and the stirring speed is 1200r/min.
5. The color masterbatch level titanium dioxide hydrophobicity detection method according to claim 4, characterized in that: in step 2), 50 to 100ml of turbid liquid is taken into a 100ml measuring cylinder.
6. The color masterbatch level titanium dioxide hydrophobicity detection method according to claim 5, characterized in that: in step 3), the wavelength of the spectrophotometer is adjusted to 680nm.
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Effective date of registration: 20220929 Address after: 618000 Xinshi Industrial Development Zone, Mianzhu City, Deyang City, Sichuan Province Applicant after: Longbai Sichuan Titanium Co.,Ltd. Applicant after: Gansu baililian Chemical Co.,Ltd. Address before: 618000 Xinshi Industrial Development Zone, Mianzhu City, Deyang City, Sichuan Province Applicant before: Longbai Sichuan Titanium Co.,Ltd. |
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