CN106940284A - A kind of dispersability of titanium dioxide detection method - Google Patents
A kind of dispersability of titanium dioxide detection method Download PDFInfo
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- CN106940284A CN106940284A CN201710373008.6A CN201710373008A CN106940284A CN 106940284 A CN106940284 A CN 106940284A CN 201710373008 A CN201710373008 A CN 201710373008A CN 106940284 A CN106940284 A CN 106940284A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N15/02—Investigating particle size or size distribution
- G01N15/0205—Investigating particle size or size distribution by optical means, e.g. by light scattering, diffraction, holography or imaging
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
Abstract
The present invention relates to a kind of detection method of dispersability of titanium dioxide, belong to the dispersed detection technique field of particulate matter, titanium dioxide, dispersant are added configuration in absolute ethyl alcohol and form detected sample by described detection method, then detected sample is subjected to ultrasonic disperse, after ultrasonic disperse titanium dioxide grain diameter measurement is carried out using laser particle analyzer, jitter time is untill particle diameter is unchanged, the D detected when laser particle analyzer50、D97And dispersion of distribution Span it is unchanged when, you can for characterizing the crystal particle diameter of titanium dioxide, when required jitter time is different, the dispersiveness of titanium dioxide is characterized with jitter time, the time is shorter, dispersiveness is better, when dispensed between it is identical, then D50Value is smaller, and dispersiveness is better, and the detection method in the present invention can measure the simple particle diameter of sample, the dispersiveness of titanium dioxide sample can truly be reflected again, cost is relatively low, and operating process is relatively simple.
Description
Technical field
The invention belongs to the dispersed detection technique field of particulate matter, and in particular to a kind of dispersability of titanium dioxide detection side
Method.
Background technology
Titanium dioxide is the most outstanding white inorganic pigment so far, and its performance is largely dependent on dioxy
Change the degree of scatter of titanium crystal particle diameter and aggregate.Because pigmentary titanium dioxide crystal particle diameter is visible wavelength half,
Submicron order, easily reunites, and the dispersiveness in titanium dioxide crystal particle diameter and different application medium is major quality controlling index.
Crystal particle diameter analysis is generally using laser particle analyzer, sedimentation particle size analyzer equigranular determining instrument and ESEM, transmission electron microscope etc.
Electron microscopic instrument.Dispersiveness detection generally uses slurrying Hegman grind gage method in coating industry, is used in plastic industry
Filter pressure and thin film testing method, use the slurrying precipitation method in chemical fibre and papermaking water-based system.
Determination of electron microscopy particle diameter is directly perceived, relatively more accurate, but statistical comparison is numerous and diverse, simultaneously because the price of instrument and making
With with high costs, electron microscope is confined to institution of higher learning and scientific research institutions, domestic titanium dioxide production enterprise and uses enterprise
It is rare.Manufacturing enterprise takes sample presentation to detect that each sample detects thousand yuan of price, and detection time is long to colleges and universities or R＆D institution, practical
Property is little；Laser particle analyzer price is relatively cheap, and method is simple and direct, and titanium white production enterprise is provided according to instrument supplier
Method, the particle diameter detected goes out greatly 2 times than the particle diameter that Electronic Speculum is detected, can neither detect real crystal particle diameter, again can not be anti-
Reflect pigmentary titanium dioxide dispersiveness.
The dispersed detecting method that current manufacturing enterprise uses, testing result is with 2 order of magnitude micron grain sizes or particle precipitation
Dispersiveness is highly characterized, differs too big with the sub-micron particle diameter of optical property requirements, it is impossible to which real reflection dispersiveness is to titanium dioxide
The influence of titanium pigment performance, can not correctly characterize dispersability of titanium dioxide, many products are distributed to 20 microns easily, but to divide
Particle diameter needed for being scattered to pigment performance is very difficult.Laser particle analyzer detection titanium dioxide powder particle diameter is generally made using calgon
Dispersant, suspension is made with distilled water, and scattered 5 minutes with ultrasonic wave, dispersion effect is bad, and the particle diameter measured, which is represented, reunites
Body.
The content of the invention
Instant invention overcomes shortcoming of the prior art, there is provided a kind of detection method of dispersability of titanium dioxide, the party
Titanium dioxide is dispersed to simple particle diameter, i.e. crystal particle diameter by method, and the dispersiveness of titanium dioxide, the party are characterized by jitter time
Method can correctly reflect the dispersiveness of titanium dioxide, and can also detect the real crystal particle diameter of titanium dioxide simultaneously.
The present invention concrete technical scheme be：
A kind of detection method of dispersability of titanium dioxide, key point is that described detection method comprises the following steps：
A, sample configuration
Titanium dioxide, dispersant are added in absolute ethyl alcohol, three's mass ratio is (2.5-5)：(5-15)：100, configure shape
Into detected sample；
B, ultrasonic disperse
Detected sample is carried out to use laser particle analyzer to carry out titanium dioxide particle diameter during ultrasonic disperse, ultrasonic disperse
Measurement, time of measuring interval is not more than 1min, ultrasonic disperse to survey titanium dioxide particle diameter it is unchanged untill and record scattered
Time；
C, combined data
Different titanium dioxide samples are operated by above-mentioned steps, are respectively obtained laser particle analyzer and are surveyed data D50、D97, point
Cloth width S pan and the jitter time needed for ultrasonic disperse；
D, interpretation of result
The D that laser particle analyzer is detected50、D97And dispersion of distribution Span is used for characterizing the crystal particle diameter of titanium dioxide；When
When the jitter time of different titanium dioxide samples is different, dispersiveness is characterized with jitter time, jitter time is shorter, and dispersiveness is got over
It is good；When the jitter time of different titanium dioxide samples is identical, with D50Value characterizes dispersiveness, D50Value is smaller, and dispersiveness is got over
It is good.
In described step A, dispersant is polyethylene glycol or monoisopropanolamine.
In described step A, the mass figures of titanium dioxide are accurate to 0.2mg.
In described step B, ultrasonic disperse device therefor is ultrasonic wave nano material disperser.
The beneficial effects of the invention are as follows：The present invention enters from factors such as selection, the jitter times of sample size, dispersant and consumption
Row is limited, and defines the dispersion condition of titanium dioxide sample, can be within the time that can be controlled and in the short period dioxy
Change titanium sample dispersion to simple particle diameter, i.e. crystal particle diameter.The titanium dioxide sample of different-grain diameter is distributed to simple particle diameter and taken
Between be different, the dispersiveness of titanium dioxide is characterized with jitter time, measuring result error can be avoided than prior art
Larger situation, and detect that obtained particle size can reflect real simple particle diameter, when there are different sample dispersions
Between it is identical when, with D50Particle size values come characterize its dispersiveness, D50The smaller dispersiveness of particle size values is better, therefore, the technology in the present invention
The simple particle diameter that scheme can measure sample can reflect the dispersiveness of sample truly, exactly again.
Embodiment
The present invention relates to a kind of detection method of dispersability of titanium dioxide, described detection method includes sample configuration, surpassed
Sound disperses and interpretation of result, certain dispersion condition by providing, by titanium dioxide sample rapid dispersion to crystal particle diameter
State, then characterizes its dispersiveness with its jitter time, and specific operating procedure is illustrated by specific embodiment, but
Present disclosure should not be confined to following embodiments, on the premise of without departing from the technology of the present invention thought category, according to
Replacement and change that common knowledge is made, belong to present disclosure.
Specific embodiment, titanium dioxide sample a, b and c of three groups of different-grain diameters of preparation, then adds three groups of samples respectively
Bonus point powder is simultaneously disperseed by the method for ultrasonic disperse, and jitter time is reported in Table 1 below, when three groups of samples are tested,
In order to ensure variable uniqueness principle, tested using identical addition and identical dispersant, dispersant selects poly- second
Glycol solution, experimentation is as follows：
Sample weighing：1.0g titanium dioxide samples are weighed, 0.2mg is accurate to；
Sample is configured：Add 20mL absolute ethyl alcohols in 50mL glass beaker, be subsequently added 2mL30g/L polyethylene glycol molten
Liquid and weighed sample, are stirred with clean glass bar, allow sample by medium complete wetting；
Ultrasonic disperse：The ultrasonic transformer of ultrasonic wave nano material disperser, ultrasonic wave are inserted in the glass for fill sample
Power is the measurement for carrying out titanium dioxide particle diameter during 10w, ultrasonic disperse using laser particle analyzer, and time of measuring interval is little
In 1min, ultrasonic disperse untill when the value for surveying sample particle diameter does not change with jitter time, record it is scattered it is required most in short-term
Between；
Detection：Scattered sample is added in ready laser particle analyzer sample introduction box, according to shading than 11~
13% control feeding quantity, tests particle diameter, obtains D50、D97And particle diameter distribution width Span value.
Data record after tri- groups of weighing sample experiments of a, b, c is as follows in table 1：
The titanium dioxide sample jitter time summary sheet of the different-grain diameter of table 1
As shown in Table 1：The time required to the titanium dioxide sample of different-grain diameter is dispersed to 0.2-0.4 μm (visible ray half-wavelength)
Difference is larger, for example：A sample particle diameters and b sample particle diameters D50Value difference 0.010, jitter time difference 2min, with jitter time come
The titanium dioxide of different-grain diameter is characterized, the dispersiveness of different samples can be substantially distinguished, dispersiveness characterizes effect preferably, therefore
It can be good at reflecting the dispersiveness of titanium dioxide with jitter time.
The titanium dioxide sample to 6 groups of unknown particle diameters carries out the detection of dispersiveness using the method for the present invention below, disperses
Constant to particle diameter, finally record surveys particle diameter and jitter time, is entered respectively using polyethylene glycol and monoisopropanolamine as dispersant
Laser particle analyzer test constantly titanium dioxide is used during the dispersion experiment of the different titanium dioxide samples of row 1-6, ultrasonic disperse
The D of titanium sample50、D97And dispersion of distribution Span values, time of measuring interval is not more than 1min, when above-mentioned numerical value is constant, ultrasound
Scattered to terminate, the jitter time needed for record ultrasonic disperse, different titanium dioxide samples pass through said process, obtain multigroup reality
Data are tested, dispersed analysis are then carried out, shown in experiment 1- experiments 6 of the detailed process as corresponding to 1-6 samples：
Experiment 1
A, sample configuration
0.5g pigmentary titanium dioxide samples are weighed, 0.2mg is accurate to, the anhydrous second of 20mL is added in 50mL glass beaker
Alcohol, then adds 2mL30g/L polyglycol solution and the titanium dioxide sample of weighing in absolute ethyl alcohol, with cleaning
Glass bar is stirred, until sample is by medium complete wetting；
B, ultrasonic disperse
The ultrasonic transformer of ultrasonic wave nano material disperser is inserted in the glass for fill sample, ultrasonic power is 10w,
The measurement of sample particle diameter is carried out using laser particle analyzer every 1min, takes titanium dioxide sample to be added to ready laser particle size
In instrument sample introduction box, according to shading than 11~13% control feeding quantities, test grain diameter measurement data include D50、D97And distribution is wide
Laser particle analyzer is surveyed numerical value and no longer changed after degree Span numerical value, scattered 10min, finally, records D50、D97And the dispersion of distribution
Span numerical value and required jitter time；
Experiment 2
A, sample configuration
0.5g pigmentary titanium dioxide samples are weighed, 0.2mg is accurate to, the anhydrous second of 20mL is added in 50mL glass beaker
Alcohol, then adds 3mL30g/L monoisopropanolamine solution and the titanium dioxide sample of weighing in absolute ethyl alcohol, with cleaning
Glass bar stirring, until sample is by medium complete wetting；
B, ultrasonic disperse
The ultrasonic transformer of ultrasonic wave nano material disperser is inserted in the glass for fill sample, ultrasonic power is 10w,
The measurement of sample particle diameter is carried out using laser particle analyzer every 1min, takes titanium dioxide sample to be added to ready laser particle size
In instrument sample introduction box, according to shading than 11~13% control feeding quantities, test grain diameter measurement data include D50、D97And distribution is wide
Laser particle analyzer is surveyed numerical value and no longer changed after degree Span numerical value, scattered 15min, finally, records D50、D97And the dispersion of distribution
Span numerical value and required jitter time；
Experiment 3
A, sample configuration
0.8g pigmentary titanium dioxide samples are weighed, 0.2mg is accurate to, the anhydrous second of 20mL is added in 50mL glass beaker
Alcohol, then adds 3mL30g/L polyglycol solution and the titanium dioxide sample of weighing in absolute ethyl alcohol, with cleaning
Glass bar is stirred, until sample is by medium complete wetting；
B, ultrasonic disperse
The ultrasonic transformer of ultrasonic wave nano material disperser is inserted in the glass for fill sample, ultrasonic power is 10w,
The measurement of sample particle diameter is carried out using laser particle analyzer every 1min, takes titanium dioxide sample to be added to ready laser particle size
In instrument sample introduction box, according to shading than 11~13% control feeding quantities, test grain diameter measurement data include D50、D97And distribution is wide
Laser particle analyzer is surveyed numerical value and no longer changed after degree Span numerical value, scattered 5min, finally, records D50、D97And the dispersion of distribution
Span numerical value and required jitter time；
Experiment 4
A, sample configuration
0.8g pigmentary titanium dioxide samples are weighed, 0.2mg is accurate to, the anhydrous second of 20mL is added in 50mL glass beaker
Alcohol, then adds 2mL30g/L monoisopropanolamine solution and the titanium dioxide sample of weighing in absolute ethyl alcohol, with cleaning
Glass bar stirring, until sample is by medium complete wetting；
B, ultrasonic disperse
The ultrasonic transformer of ultrasonic wave nano material disperser is inserted in the glass for fill sample, ultrasonic power is 10w,
The measurement of sample particle diameter is carried out using laser particle analyzer every 1min, takes titanium dioxide sample to be added to ready laser particle size
In instrument sample introduction box, according to shading than 11~13% control feeding quantities, test grain diameter measurement data include D50、D97And distribution is wide
Laser particle analyzer is surveyed numerical value and no longer changed after degree Span numerical value, scattered 10min, finally, records D50、D97And the dispersion of distribution
Span numerical value and required jitter time；
Experiment 5
A, sample configuration
1.0g pigmentary titanium dioxide samples are weighed, 0.2mg is accurate to, the anhydrous second of 20mL is added in 50mL glass beaker
Alcohol, then adds 1mL30g/L polyglycol solution and the titanium dioxide sample of weighing in absolute ethyl alcohol, with cleaning
Glass bar is stirred, until sample is by medium complete wetting；
B, ultrasonic disperse
The ultrasonic transformer of ultrasonic wave nano material disperser is inserted in the glass for fill sample, ultrasonic power is 10w,
The measurement of sample particle diameter is carried out using laser particle analyzer every 1min, takes titanium dioxide sample to be added to ready laser particle size
In instrument sample introduction box, according to shading than 11~13% control feeding quantities, test grain diameter measurement data include D50、D97And distribution is wide
Laser particle analyzer is surveyed numerical value and no longer changed after degree Span numerical value, scattered 15min, finally, records D50、D97And the dispersion of distribution
Span numerical value and required jitter time；
Experiment 6
A, sample configuration
1.0g pigmentary titanium dioxide samples are weighed, 0.2mg is accurate to, the anhydrous second of 20mL is added in 50mL glass beaker
Alcohol, then adds 2mL30g/L monoisopropanolamine solution and the titanium dioxide sample of weighing in absolute ethyl alcohol, with cleaning
Glass bar stirring, until sample is by medium complete wetting；
B, ultrasonic disperse
The ultrasonic transformer of ultrasonic wave nano material disperser is inserted in the glass for fill sample, ultrasonic power is 10w,
The measurement of sample particle diameter is carried out using laser particle analyzer every 1min, takes titanium dioxide sample to be added to ready laser particle size
In instrument sample introduction box, according to shading than 11~13% control feeding quantities, test grain diameter measurement data include D50、D97And distribution is wide
Laser particle analyzer is surveyed numerical value and no longer changed after degree Span numerical value, scattered 5min, finally, records D50、D97And the dispersion of distribution
Span numerical value and required jitter time；
The particle size data and jitter time of different samples are obtained according to experiment 1-9 records, all data summarizations into table 2,
It is as shown in the table：
The experimental result data of table 2
Test in 1-6, the conduct with monoisopropanolamine, the existing titanium dioxide of polyethylene glycol replacement conventional calgon
Dispersant, compared to existing calgon for the dispersion effect of titanium dioxide, but triisopropanolamine or poly- second two
Alcohol can make titanium dioxide be dispersed to simple particle diameter by the ultrasonic disperse of short period so that dispersability of titanium dioxide characterizes institute
Take time and greatly shorten, and result in the simple particle diameter of each sample, a detection process can realize two functions, into
Originally it can control in reduced levels, detection function is enriched, also, the operation that this method is detected for dispersability of titanium dioxide
Technical requirements are relatively low.
Knowable to table 2 records data：Test 3,6 jitter times most short, be 5min, the dispersiveness of titanium dioxide sample used
Preferably, in two experiments, the D of experiment 650Value is minimum, and dispersiveness preferably, take second place by experiment 3；Test 1,4 jitter times placed in the middle, be
10min, the dispersiveness of titanium dioxide sample used is not as experiment 3,6, in the two experiments, the D of experiment 150Value is minimum, dispersiveness
Preferably, experiment 4 is taken second place；Test 2,5 jitter times it is most long, be 15min, titanium dioxide sample used it is dispersed worst, at this
In two experiments, the D of experiment 550Value is minimum, and dispersiveness preferably, take second place by experiment 2.There is above-mentioned analysis process to obtain testing 1-6
In titanium dioxide sample used dispersiveness sequence, dispersiveness by well to it is bad be ordered as experiment 6, experiment 3, experiment 1, test 4,
Experiment 5, experiment 2.
Dispersed detection method in the present invention can more accurately distinguish the dispersiveness of titanium dioxide, applied to pigment
, being capable of influence of the accurate instruction dispersiveness to TiO 2 pigment performance, the process letter of detection method with titanium dioxide sample
Single, easy to operate, cost is relatively low, can either realize the accurate characterization of dispersiveness, and the different titanium dioxides of low cost can be realized again
The crystal particle diameter detection of titanium sample, in addition, this method can also be widely used in the phase in the industries such as plastics, chemical fibre and papermaking
The detection of dispersiveness is closed, application field is relatively broad.
Claims (4)
1. a kind of detection method of dispersability of titanium dioxide, it is characterised in that described detection method comprises the following steps：
A, sample configuration
Titanium dioxide, dispersant are added in absolute ethyl alcohol, three's mass ratio is (2.5-5)：(5-15)：100, configuration formation is treated
Detect sample；
B, ultrasonic disperse
The survey that detected sample is carried out using laser particle analyzer to carry out titanium dioxide particle diameter during ultrasonic disperse, ultrasonic disperse
Amount, time of measuring interval is not more than 1min, ultrasonic disperse to survey titanium dioxide particle diameter it is unchanged untill and record jitter time；
C, combined data
Different titanium dioxide samples are operated by above-mentioned steps, are respectively obtained laser particle analyzer and are surveyed data D50、D97, the dispersion of distribution
Span and the jitter time needed for ultrasonic disperse；
D, interpretation of result
The D that laser particle analyzer is detected50、D97And dispersion of distribution Span is used for characterizing the crystal particle diameter of titanium dioxide；Work as difference
When the jitter time of titanium dioxide sample is different, dispersiveness is characterized with jitter time, jitter time is shorter, dispersiveness is better；
When the jitter time of different titanium dioxide samples is identical, with D50Value characterizes dispersiveness, D50Value is smaller, and dispersiveness is better.
2. a kind of detection method of dispersability of titanium dioxide according to claim 1, it is characterised in that described step A
In, dispersant is polyethylene glycol or monoisopropanolamine.
3. a kind of detection method of dispersability of titanium dioxide according to claim 1, it is characterised in that described step A
In, the mass figures of titanium dioxide are accurate to 0.2mg.
4. a kind of detection method of dispersability of titanium dioxide according to claim 1, it is characterised in that described step B
In, ultrasonic disperse device therefor is ultrasonic wave nano material disperser.
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| CN108760586A (en) * | 2018-05-23 | 2018-11-06 | 广州能源检测研究院 | A kind of method that overlay material particle size is distributed in detection lithium battery pole slice |
| CN109580436A (en) * | 2019-01-02 | 2019-04-05 | 云南大学 | Dispersion performance characterizing method for the dispersing agent in casting slurry preparation process |
| CN111044414A (en) * | 2019-11-26 | 2020-04-21 | 天能电池集团股份有限公司 | Method for detecting particle size of colloidal graphite for lead storage battery |
| CN112858115A (en) * | 2021-01-14 | 2021-05-28 | 重庆大学 | Method for detecting dispersibility of nano material |
| CN112858075A (en) * | 2021-02-08 | 2021-05-28 | 中冶长天国际工程有限责任公司 | Method for detecting kneading effect of multi-component raw materials |
| CN113447405A (en) * | 2020-03-26 | 2021-09-28 | 北京橡胶工业研究设计院有限公司 | Microcrystalline graphite particle size testing method |
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| CN114184523B (en) * | 2022-02-14 | 2022-05-03 | 徐州钛白化工有限责任公司 | Method for detecting titanium dioxide dispersibility |
| CN114716873A (en) * | 2022-05-10 | 2022-07-08 | 烟台金桥优尼科新材料科技有限公司 | Carrier solution of titanium dioxide and rapid evaluation method for dispersibility of titanium dioxide |
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Application publication date: 20170711 |