CN105259130B - A kind of method for detecting titanium dioxide surface organic process stability - Google Patents
A kind of method for detecting titanium dioxide surface organic process stability Download PDFInfo
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- CN105259130B CN105259130B CN201510844220.7A CN201510844220A CN105259130B CN 105259130 B CN105259130 B CN 105259130B CN 201510844220 A CN201510844220 A CN 201510844220A CN 105259130 B CN105259130 B CN 105259130B
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Abstract
The invention belongs to chemical technology field, and in particular to a kind of method for detecting titanium dioxide surface organic process stability.The technical problems to be solved by the invention are to provide a kind of method for detecting titanium dioxide surface organic process stability, comprise the following steps：A, titanium dioxide three is washed into the gentle powder of material drying to constant weight；B, detected with infrared spectrometer；C, the difference for comparing every batch of gas powder and three infrared spectrums for washing material is composed；D, by organic agent, drying to constant weight, its whole element with energy disperse spectroscopy qualitative detection；E, the three each elements for washing material and every batch of gas powder are quantitatively detected with elemental analyser；If f, every batch of gas powder is washed some constituent content difference of material with three and differed, i.e. the dosage of the organic agent is unstable；If difference is identical, this kind of element dosage is stablized.The method of the present invention has the directive significance of feedback regulation to improving organic agent adding technology.
Description
Technical field
The invention belongs to chemical technology field, and in particular to a kind of side for detecting titanium dioxide surface organic process stability
Method.
Background technology
Titanium dioxide is important inorganic functional material, because it has unique physics, chemical property, is widely used in
The industries such as coating, plastics, papermaking, ink, chemical fibre, rubber, cosmetics.Organic process improves titanium dioxide and resin and organic
The compatibility of solvent, so as to improve the application performance of titanium dioxide.
Reported according to current pertinent literature, organic agent adds in dry and air-flow crushing two procedures in industrial production
Add, adsorbed in a manner of physically or chemically on titanium dioxide surface.The suction type and the uniform and stable property shadow of addition of organic agent
Ring the dispersiveness to titanium dioxide, the stability of oil absorption, and the index such as covering power.
In the detection technique for the organic surface treatment effect of titanium dioxide being related to, there has been no on organic surface treatment effect
Effective verification method.Using this method by detecting the suction type of organic agent and the stability of additive amount, there is effect
Demonstrate,prove the stability of titanium dioxide surface organic process effect.
The content of the invention
For the technological deficiency in existing field, it is organic that goal of the invention of the invention is to provide a kind of detection titanium dioxide surface
The method of Treatment Stability.
The technical problems to be solved by the invention are to provide a kind of method for detecting titanium dioxide surface organic process stability.
This method comprises the following steps：
A, wash material by more than a batch three and distinguished by the gas powder that every batch of three is washed more than two batches for expecting to be prepared
Drying to constant weight；
B, detect that drying to constant weight respectively with infrared spectrometer three wash the gentle powder of material, respectively obtain respective infrared light
Spectrogram；
C, it is compared according to above-mentioned infrared spectrogram, obtains a certain batch three and wash material and every batch of gas prepared therefrom
The poor spectrogram of powder；It is variant that if these differences compose mutual characteristic peak positions, then it is assumed that titanium dioxide surface organic process is not
Stablize；If these differences, which compose mutual characteristic peak positions, does not have difference, then carries out step d；
Or be compared according to above-mentioned infrared spectrogram, obtain a certain batch three and wash material and every batch of prepared therefrom
The poor spectrogram and another batch three of gas powder wash the poor spectrogram of material and every batch of gas powder prepared therefrom；If these are poor
It is variant to compose mutual characteristic peak positions, then it is assumed that titanium dioxide surface organic process is unstable；If these difference spectrum mutually it
Between characteristic peak positions there is no difference, then carry out step d；
D, by organic agent, drying to constant weight, its whole element with energy disperse spectroscopy qualitative detection；
E, the element according to contained by the organic agent that step d is measured, then quantitatively detect that drying to constant weight respectively three wash
Expect in gentle powder with the corresponding element contained by organic agent；
F, analyzed, removed outside detection error according to the data of step e, obtained a certain batch three and wash material with being prepared by it
Every batch of gas powder in each constituent content difference；If each constituent content difference all same, then it is assumed that titanium dioxide table
Face organic process is stablized；If there is a constituent content difference difference, then it is assumed that titanium dioxide surface organic process is unstable；
Or analyzed according to the data of step e, remove outside error-detecting, obtain a certain batch and gas prepared therefrom
Each constituent content difference and another batch three wash material and each constituent content in gas powder prepared therefrom in powder
Difference；If each constituent content difference all same, then it is assumed that titanium dioxide surface organic process is stablized；If there is a constituent content
Difference is different, then it is assumed that titanium dioxide surface organic process is unstable.
Preferably, the method for above-mentioned detection titanium dioxide surface organic process stability, comprises the following steps：
A, a certain batch three of titanium dioxide is washed into material and gas powders more than two batches for expecting to be prepared is washed by the batch three
It is respectively dried to constant weight；
B, detect that drying to constant weight respectively with infrared spectrometer three wash the gentle powder of material, respectively obtain respective infrared light
Spectrogram；
C, it is compared according to above-mentioned infrared spectrogram, obtains the batch three and wash material and every batch of gas powder prepared therefrom
The poor spectrogram of material；It is variant that if these differences compose mutual characteristic peak positions, then it is assumed that titanium dioxide surface organic process is unstable
It is fixed；If these differences, which compose mutual characteristic peak positions, does not have difference, then carries out step d；
D, by organic agent, drying to constant weight, its whole element with energy disperse spectroscopy qualitative detection；
E, the element according to contained by the organic agent that step d is measured, then quantitatively detect that drying to constant weight respectively three wash
Expect in gentle powder with the corresponding element contained by organic agent；
F, analyzed according to the data of step e, remove detection error outside, obtain the batch three wash material with it is prepared therefrom
Each constituent content difference in every batch of gas powder；If each constituent content difference all same, then it is assumed that titanium dioxide surface
Organic process is stablized；If there is a constituent content difference difference, then it is assumed that titanium dioxide surface organic process is unstable.
Preferably, in the method and step a of above-mentioned detection titanium dioxide surface organic process dosage stability, the drying temperature
Spend for 105~120 DEG C, the time is 24~36h.
Preferably, in the method and step b of above-mentioned detection titanium dioxide surface organic process dosage stability, infrared spectrometer pressure
The ︰ 20~25 of Dai test samples Pin ︰ potassium bromide=1 in mass ratio during piece.
Preferably, in the method and step d of above-mentioned detection titanium dioxide surface organic process dosage stability, the drying temperature
Spend for 105~110 DEG C, the time is 4~8h.
Preferably, in the method and step e of above-mentioned detection titanium dioxide surface organic process dosage stability, the quantitative inspection
Survey to 100ppm.
The method of the present invention is added by having effectively monitored different batches in production process with trade mark product organic agent
Uniformity and stability, effective quantitative analysis has been carried out to the unstable reason such as the dispersiveness of titanium dioxide.Organic agent
Dosage is stablized, then ensure that the stabilization of titanium dioxide dispersiveness, oil absorption and application performance；A certain element dosage shakiness rule is led
The unstable of titanium dioxide dispersiveness etc. is caused, then seriously affects the product quality of titanium dioxide.To improving organic agent adding technology
There is the directive significance of feedback regulation.
Embodiment
A kind of method for detecting titanium dioxide surface organic process stability, comprises the following steps：
A, wash material by more than a batch three and distinguished by the gas powder that every batch of three is washed more than two batches for expecting to be prepared
Drying to constant weight；
B, detect that drying to constant weight respectively with infrared spectrometer three wash the gentle powder of material, respectively obtain respective infrared light
Spectrogram；
C, it is compared according to above-mentioned infrared spectrogram, obtains a certain three and wash material and every batch of gas powder prepared therefrom
Poor spectrogram；It is variant that if all differences compose mutual characteristic peak positions, then it is assumed that titanium dioxide surface organic process is unstable；
If all differences, which compose mutual characteristic peak positions, does not have difference, then carries out step d；
Or be compared according to above-mentioned infrared spectrogram, obtain this three wash material with every batch of gas powder prepared therefrom
Poor spectrogram and that three wash material and the poor spectrogram of every batch of gas powder prepared therefrom；If difference composes mutual characteristic peak positions
It is variant, then it is assumed that titanium dioxide surface organic process is unstable；If difference, which composes mutual characteristic peak positions, does not have difference, then into
Row step d；
D, by organic agent, drying to constant weight, its whole element with energy disperse spectroscopy qualitative detection；
E, the element according to contained by the organic agent that step d is measured, then quantitatively detect that drying to constant weight respectively three wash
Expect in gentle powder with the corresponding element contained by organic agent；
F, analyzed, removed outside detection error according to the data of step e, if a certain three wash material and every batch of prepared therefrom
Each constituent content difference all same in secondary gas powder, then it is assumed that titanium dioxide surface organic process is stablized；If three wash material with it is every
There is a constituent content difference to differ in batch gas powder, then it is assumed that titanium dioxide surface organic process is unstable；
Or analyzed according to the data of step e, remove error-detecting outside, if this three wash material with gas powder prepared therefrom
In material each constituent content difference with that three wash material with gas powder prepared therefrom in each constituent content difference all same,
Then think that titanium dioxide surface organic process is stablized；If this three wash material with gas powder prepared therefrom in each constituent content difference
With that three wash material with thering is a constituent content difference to differ in gas powder prepared therefrom, then it is assumed that the organic place in titanium dioxide surface
Manage unstable.
Preferably, the method for above-mentioned titanium dioxide surface organic process dosage stability, comprises the following steps：
A, a certain batch three of titanium dioxide is washed into material and gas powders more than two batches for expecting to be prepared is washed by the batch three
It is respectively dried to constant weight；
B, detect that drying to constant weight respectively with infrared spectrometer three wash the gentle powder of material, respectively obtain respective infrared light
Spectrogram；
C, compare three infrared spectrograms for washing material and every batch of gas powder, respectively obtain three and wash material and every batch of gas powder
Infrared light spectral difference is composed；If all difference spectrums are variant between each other, then it is assumed that titanium dioxide surface organic process is unstable；If institute
There is difference spectrum there is no difference between each other, then carry out step d；
D, by organic agent, drying to constant weight, its whole element with energy disperse spectroscopy qualitative detection；
E, the element according to contained by the organic agent that step d is measured, then quantitatively detection is dried respectively with elemental analyser
To the three of constant weight wash in the gentle powder of material with the corresponding element contained by organic agent；
F, analyzed according to the data of step e, if three wash material and each constituent content difference in every batch of gas powder
All same, then it is assumed that titanium dioxide surface organic process is stablized；If three wash material with there is a constituent content poor in every batch of gas powder
Value differs, then it is assumed that titanium dioxide surface organic process is unstable.
Organic agent described in the method for the present invention be in titanium dioxide surface treatment, titanium dioxide surface is carried out physics or
Chemical modification, improves the dispersiveness and application performance of titanium dioxide, generally there is polyalcohols, organic silicon or amine.
Above-mentioned example embodiment for a better understanding of the present invention, carries out further it with reference to specific example
Explanation.
The infrared spectrometer that the embodiment of the present invention uses flies IS50 Fourier transform infrared spectroscopies to match to write from memory；Si is analyzed to use
Atomic Absorption Spectrometer AA800, accuracy of detection 100ppm；Analysis C uses CS analyzers CS2000.
Embodiment 1
Same dosage is pressed with organic silicon emulsion A, the same a collection of inorganic coating material of rutile type titanium white is surface-treated, does two
The parallel examination 1# and 2# of group, it is respectively 0.095 and 0.249,1# to measure C and Si percentage compositions in before processing titanium dioxide according to the present invention
Containing being respectively 0.160 and 0.280, the difference spectrum of its infrared spectrum shows C-H in 2850cm for number gas powder C and Si percentage-1~
3000cm-1Between have obvious absworption peak；2# gas powder C and Si percentage compositions are respectively 0.158 and 0.250, and same its is red
The difference spectrum of external spectrum shows C-H in 2850cm-1~3000cm-1Between obvious absworption peak.
From the present embodiment data can be seen that infrared spectrum difference spectrum it is identical, the change of C is identical, then is considered as titanium white
C is stable during the organic process of powder surface；And the change of Si is different, then it is not to be considered as Si during the organic process of titanium dioxide surface
Stable, so as to judge that titanium dioxide surface organic process is unstable.
Embodiment 2
Same dosage is pressed with organic silicon emulsion B, the same a collection of inorganic coating material of rutile type titanium white is surface-treated, does two
The parallel examination 1# and 2# of group, C and Si percentages are measured in before processing titanium dioxide containing respectively 0.095 and 0.240, No. 1# according to the present invention
Gas powder C and Si percentage composition is respectively 0.148 and 0.281, and the difference spectrum of its infrared spectrum shows C-H in 2850cm-1~
3000cm-1Between have obvious absworption peak；C-H2# gas powder C and Si percentage compositions are respectively 0.150 and 0.288, it is same its
The difference spectrum of infrared spectrum shows C-H in 2850cm-1~3000cm-1Between have obvious absworption peak.
Can be seen that the difference spectrum of infrared spectrum is identical from the present embodiment data, identical, Si the change of change of C is also identical,
It is judged that C and Si is stable during the organic process of titanium dioxide surface, so as to judge that titanium dioxide surface organic process is steady
Fixed.
Evaluation method provided by the invention has good in terms of organic surface treatment of the inorganic pigments such as titanium dioxide and filler
Good application and promotion prospect.
Claims (6)
- A kind of 1. method for detecting titanium dioxide surface organic process stability, it is characterised in that：Comprise the following steps：A, wash material by more than a batch three and be respectively dried by the gas powder that every batch of three is washed more than two batches for expecting to be prepared To constant weight；B, detect that drying to constant weight respectively with infrared spectrometer three wash the gentle powder of material, respectively obtain respective infrared spectrum Figure；C, it is compared according to above-mentioned infrared spectrogram, obtains a certain batch three and wash material and every batch of gas powder prepared therefrom Poor spectrogram；It is variant that if these differences compose mutual characteristic peak positions, then it is assumed that titanium dioxide surface organic process is unstable； If these differences, which compose mutual characteristic peak positions, does not have difference, then carries out step d；Or be compared according to above-mentioned infrared spectrogram, obtain a certain batch three and wash material and every batch of gas powder prepared therefrom The poor spectrogram and another batch three of material wash the poor spectrogram of material and every batch of gas powder prepared therefrom；If these difference spectrum phases Characteristic peak positions are variant between mutually, then it is assumed that titanium dioxide surface organic process is unstable；If these difference spectrums are special between each other Sign peak position does not have difference, then carries out step d；D, by organic agent, drying to constant weight, its whole element with energy disperse spectroscopy qualitative detection；E, the element according to contained by the organic agent that step d is measured, then quantitatively detect that drying to constant weight respectively three wash material and In gas powder with the corresponding element contained by organic agent；F, analyzed, removed outside detection error according to the data of step e, obtain a certain batch three wash material with it is prepared therefrom every Each constituent content difference in batch gas powder；If each constituent content difference all same, then it is assumed that titanium dioxide surface has Machine processing is stablized；If there is a constituent content difference difference, then it is assumed that titanium dioxide surface organic process is unstable；Or analyzed according to the data of step e, remove outside error-detecting, obtain a certain batch and gas powder prepared therefrom In each constituent content difference and another batch three to wash material poor with each constituent content in gas powder prepared therefrom Value；If each constituent content difference all same, then it is assumed that titanium dioxide surface organic process is stablized；If there is the constituent content poor Value is different, then it is assumed that titanium dioxide surface organic process is unstable.
- 2. the method for detection titanium dioxide surface according to claim 1 organic process stability, it is characterised in that：Including with Lower step：A, a certain batch three of titanium dioxide is washed into material and is distinguished by the gas powder that the batch three is washed more than two batches for expecting to be prepared Drying to constant weight；B, detect that drying to constant weight respectively with infrared spectrometer three wash the gentle powder of material, respectively obtain respective infrared spectrum Figure；C, it is compared according to above-mentioned infrared spectrogram, obtains the batch three and wash material and every batch of gas powder prepared therefrom Poor spectrogram；It is variant that if these differences compose mutual characteristic peak positions, then it is assumed that titanium dioxide surface organic process is unstable；Such as These differences of fruit, which compose mutual characteristic peak positions, does not have difference, then carries out step d；D, by organic agent, drying to constant weight, its whole element with energy disperse spectroscopy qualitative detection；E, the element according to contained by the organic agent that step d is measured, then quantitatively detect that drying to constant weight respectively three wash material and In gas powder with the corresponding element contained by organic agent；F, analyzed, removed outside detection error according to the data of step e, obtained the batch three and wash material and every batch of prepared therefrom Each constituent content difference in secondary gas powder；If each constituent content difference all same, then it is assumed that titanium dioxide surface is organic Processing is stablized；If there is a constituent content difference difference, then it is assumed that titanium dioxide surface organic process is unstable.
- 3. the method for detection titanium dioxide surface according to claim 1 or 2 organic process stability, it is characterised in that：Step In rapid a, the drying temperature is 105~120 DEG C, and the time is 24~36h.
- 4. in the method and step b of detection titanium dioxide surface according to claim 1 or 2 organic process stability, infrared light The ︰ 20~25 of Dai test samples Pin ︰ potassium bromide=1 in mass ratio during spectrometer tabletting.
- It is 5. described in the method and step d of detection titanium dioxide surface according to claim 1 or 2 organic process stability Drying temperature is 105~110 DEG C, and the time is 4~8h.
- It is 6. described in the method and step e of detection titanium dioxide surface according to claim 1 or 2 organic process stability It is quantitative to detect to 100ppm.
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| CN107817316A (en) * | 2017-10-30 | 2018-03-20 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of detection method of titanium dioxide organic silicon emulsion ph stability |
| CN107656024B (en) * | 2017-11-13 | 2019-11-22 | 龙蟒佰利联集团股份有限公司 | A kind of measuring method of titanium dioxide surface organosilicon stearic acid organic agent covering amount |
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