CN105259130A - Method for detecting organic treatment stability of surface of titanium dioxide - Google Patents

Method for detecting organic treatment stability of surface of titanium dioxide Download PDF

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CN105259130A
CN105259130A CN201510844220.7A CN201510844220A CN105259130A CN 105259130 A CN105259130 A CN 105259130A CN 201510844220 A CN201510844220 A CN 201510844220A CN 105259130 A CN105259130 A CN 105259130A
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titanium dioxide
batch
organic process
gas powder
think
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CN105259130B (en
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刘婵
李礼
杜剑桥
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Sichuan Pan Yan Technology Co., Ltd.
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Pangang Group Panzhihua Iron and Steel Research Institute Co Ltd
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Abstract

The invention belongs to the technical field of chemical engineering, and particularly relates to a method for detecting the organic treatment stability of the surface of titanium dioxide. The method comprises the following steps that a, a titanium dioxide triple-washing material and gas powder are dried to reach the constant weight; b, an infrared spectrometer is used for detection; c, differential spectra of infrared spectra of the gas powder of each batch and the triple-washing material are compared; d, an organic treatment agent is dried to reach the constant weight, and an energy disperse spectroscopy is used for qualitatively detecting all elements; e, an element analyzer is used for qualitatively detecting all the elements of the triple-washing material and the gas powder material of each batch; f, if the differences between the gas powder materials of the batches and the content of a certain element of the triple-washing material are different, the added amount of the organic treatment agent is not stable; if the differences are the same, the added amount of the elements is stable. The method has the guiding significance of feedback regulation of improving the organic treatment agent addition technology.

Description

A kind of method detecting titanium dioxide surface organic process stability
Technical field
The invention belongs to chemical technology field, be specifically related to a kind of method detecting titanium dioxide surface organic process stability.
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 the compatibility of titanium dioxide and resin and organic solvent, thus improves the application performance of titanium dioxide.
According to current pertinent literature report, in commercial production, organic agent adds in dry and air-flow crushing two procedures, is adsorbed on titanium dioxide surface in the mode of physics or chemistry.The suction type of organic agent and add the dispersiveness that uniform and stable property has influence on titanium dioxide, the stability of oil absorption, and the index such as covering power.
In the detection technique of the organic surface treatment effect of the titanium dioxide related to, not yet there is the effective verification method about organic surface treatment effect.Adopt this method by detecting the suction type of organic agent and the stability of addition, effectively the stability of checking titanium dioxide surface organic process effect.
Summary of the invention
For the technological deficiency in existing field, goal of the invention of the present invention is to provide a kind of method detecting titanium dioxide surface organic process stability.
Technical matters to be solved by this invention is to provide a kind of method detecting titanium dioxide surface organic process stability.The method comprises the following steps:
A, more than one batch three is washed material and wash by every batch three and expect that the gas powder of more than two batches prepared is dried respectively to constant weight;
B, with infrared spectrometer detect respectively dry to three of constant weight wash material gentle powder, obtain respective infrared spectrogram respectively;
C, to compare according to above-mentioned infrared spectrogram, obtain the poor spectrogram that a certain batch three is washed material and every batch of gas powder prepared therefrom; If it is variant that these differences compose characteristic peak positions each other, then think that titanium dioxide surface organic process is unstable; If these differences compose characteristic peak positions each other do not have difference, then carry out steps d;
Or compare according to above-mentioned infrared spectrogram, obtain a certain batch three and wash material and the poor spectrogram of every batch of gas powder prepared therefrom and another batch three and wash and expect and the poor spectrogram of every batch of gas powder prepared therefrom; If it is variant that these differences compose characteristic peak positions each other, then think that titanium dioxide surface organic process is unstable; If these differences compose characteristic peak positions each other do not have difference, then carry out steps d;
D, by organic agent dry to constant weight, with its whole element of energy spectrometer qualitative detection;
E, the element contained by organic agent recorded according to steps d, more quantitatively detect respectively dry to three of constant weight wash in the gentle powder of material to the corresponding element contained by organic agent;
F, data analysis according to step e, outside removing metrical error, obtain a certain batch three and wash material and each constituent content difference in every batch of gas powder prepared therefrom; If each constituent content difference is all identical, then think that titanium dioxide surface organic process is stablized; If there is a constituent content difference different, then think that titanium dioxide surface organic process is unstable;
Or according to the data analysis of step e, outside removing error-detecting, obtain a certain batch and to wash with each constituent content difference and another batch three in gas powder prepared therefrom and expect and each constituent content difference in gas powder prepared therefrom; If each constituent content difference is all identical, then think that titanium dioxide surface organic process is stablized; If there is a constituent content difference different, then think 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 for titanium dioxide batch three is washed material and washed by this batch three and expect that the gas powder of more than two batches prepared is dried respectively to constant weight;
B, with infrared spectrometer detect respectively dry to three of constant weight wash material gentle powder, obtain respective infrared spectrogram respectively;
C, to compare according to above-mentioned infrared spectrogram, obtain the poor spectrogram that this batch three washes material and every batch of gas powder prepared therefrom; If it is variant that these differences compose characteristic peak positions each other, then think that titanium dioxide surface organic process is unstable; If these differences compose characteristic peak positions each other do not have difference, then carry out steps d;
D, by organic agent dry to constant weight, with its whole element of energy spectrometer qualitative detection;
E, the element contained by organic agent recorded according to steps d, more quantitatively detect respectively dry to three of constant weight wash in the gentle powder of material to the corresponding element contained by organic agent;
F, data analysis according to step e, outside removing metrical error, obtain this batch three and wash each constituent content difference in material and every batch of gas powder prepared therefrom; If each constituent content difference is all identical, then think that titanium dioxide surface organic process is stablized; If there is a constituent content difference different, then think that titanium dioxide surface organic process is unstable.
Preferably, in the method step a of above-mentioned detection titanium dioxide surface organic process dosage stability, described bake out temperature is 105 ~ 120 DEG C, and the time is 24 ~ 36h.
Preferably, in the method step b of above-mentioned detection titanium dioxide surface organic process dosage stability, Dai test sample Pin ︰ potassium bromide=1 ︰ 20 ~ 25 in mass ratio during infrared spectrometer compressing tablet.
Preferably, in the method step d of above-mentioned detection titanium dioxide surface organic process dosage stability, described bake out temperature is 105 ~ 110 DEG C, and the time is 4 ~ 8h.
Preferably, in the method step e of above-mentioned detection titanium dioxide surface organic process dosage stability, described quantitative detection is to 100ppm.
The inventive method, by homogeneity that effectively to have monitored different batches in production run and add with trade mark product organic agent and stability, has carried out effective quantitative analysis to unstable reasons such as the dispersivenesses of titanium dioxide.Organic agent dosage is stablized, then ensure that titanium dioxide is dispersed, oil absorption and application performance stable; The unstable rule of a certain element dosage causes the instability of titanium dioxide dispersiveness etc., then have a strong impact on the product quality of titanium dioxide.The directive significance of feedback regulation is had to improving organic agent adding technology.
Embodiment
Detect a method for titanium dioxide surface organic process stability, comprise the following steps:
A, more than one batch three is washed material and wash by every batch three and expect that the gas powder of more than two batches prepared is dried respectively to constant weight;
B, with infrared spectrometer detect respectively dry to three of constant weight wash material gentle powder, obtain respective infrared spectrogram respectively;
C, to compare according to above-mentioned infrared spectrogram, obtain the poor spectrogram that a certain three wash material and every batch of gas powder prepared therefrom; If it is variant that all differences compose characteristic peak positions each other, then think that titanium dioxide surface organic process is unstable; If all differences compose characteristic peak positions each other do not have difference, then carry out steps d;
Or compare according to above-mentioned infrared spectrogram, obtain this and three wash material and the poor spectrogram of every batch of gas powder prepared therefrom and that three are washed and expect and the poor spectrogram of every batch of gas powder prepared therefrom; If it is variant that difference composes characteristic peak positions each other, then think that titanium dioxide surface organic process is unstable; If difference composes characteristic peak positions each other do not have difference, then carries out steps d;
D, by organic agent dry to constant weight, with its whole element of energy spectrometer qualitative detection;
E, the element contained by organic agent recorded according to steps d, more quantitatively detect respectively dry to three of constant weight wash in the gentle powder of material to the corresponding element contained by organic agent;
F, data analysis according to step e, outside removing metrical error, if a certain three to wash material all identical with each constituent content difference in every batch of gas powder prepared therefrom, then think that titanium dioxide surface organic process is stable; If three wash material and have a constituent content difference not identical in every batch of gas powder, then think that titanium dioxide surface organic process is unstable;
Or according to the data analysis of step e, outside removing error-detecting, if this three wash material and each constituent content difference in gas powder prepared therefrom with that three wash expect and in gas powder prepared therefrom each constituent content difference all identical, then think that the surperficial organic process of titanium dioxide is stable; If this three washes material and each constituent content difference in gas powder prepared therefrom and three wash with that and expect and have a constituent content difference not identical in gas powder prepared therefrom, then think the surperficial organic process instability of titanium dioxide.
Preferably, the method for above-mentioned titanium dioxide surface organic process dosage stability, comprises the following steps:
A, a certain for titanium dioxide batch three is washed material and washed by this batch three and expect that the gas powder of more than two batches prepared is dried respectively to constant weight;
B, with infrared spectrometer detect respectively dry to three of constant weight wash material gentle powder, obtain respective infrared spectrogram respectively;
C, compare three and wash material and the infrared spectrogram of every batch of gas powder, obtain three respectively and wash material and compose with the infrared light spectral differences of every batch of gas powder; If all difference spectrums are variant each other, then think that titanium dioxide surface organic process is unstable; If all difference spectrums do not have difference each other, then carry out steps d;
D, by organic agent dry to constant weight, with its whole element of energy spectrometer qualitative detection;
E, the element contained by organic agent recorded according to steps d, then with elemental analyser quantitatively detect respectively dry to three of constant weight wash in the gentle powder of material to the corresponding element contained by organic agent;
F, data analysis according to step e, if three to wash material all identical with each constituent content difference in every batch of gas powder, then think that titanium dioxide surface organic process is stable; If three wash material and have a constituent content difference not identical in every batch of gas powder, then think that titanium dioxide surface organic process is unstable.
Organic agent described in the inventive method is in titanium dioxide surface treatment, carries out physics or chemical modification to titanium dioxide surface, improves dispersiveness and the application performance of titanium dioxide, generally has polyalcohols, silicone based or amine.
In order to understand above-mentioned exemplary embodiment of the present invention better, below in conjunction with concrete example, it is further described.
The infrared spectrometer that the embodiment of the present invention adopts flies IS50 Fourier transform infrared spectroscopy for match is silent; Analyze Si and adopt Atomic Absorption Spectrometer AA800, accuracy of detection is 100ppm; Analyze C and adopt CS analyser CS2000.
Embodiment 1
With organic silicon emulsion A by same dosage, the same a collection of inorganic coating material of surface treatment rutile type titanium white, be two groups of parallel examination 1# and 2#, before recording process according to the present invention, in titanium dioxide, C and Si percentage composition is respectively 0.095 and 0.249,1# gas powder C and Si percentage are containing being respectively 0.160 and 0.280, and the bright C-H of poor stave of its infrared spectrum is at 2850cm -1~ 3000cm -1between have obvious absorption peak; 2# gas powder C and Si percentage composition are respectively 0.158 and 0.250, and the bright C-H of poor stave of its infrared spectrum is at 2850cm equally -1~ 3000cm -1between obvious absorption peak.
As can be seen from the present embodiment data, infrared spectrum difference spectrum identical, the change of C is identical, so just think titanium dioxide surface organic process time C be stable; And the change of Si is different, so just think titanium dioxide surface organic process time Si be unstable, thus judge that titanium dioxide surface organic process is unstable.
Embodiment 2
With organic silicon emulsion B by same dosage, the same a collection of inorganic coating material of surface treatment rutile type titanium white, be two groups of parallel examination 1# and 2#, C and Si percentage is recorded before process in titanium dioxide containing being respectively 0.095 and 0.240 according to the present invention, 1# gas powder C and Si percentage composition are respectively 0.148 and 0.281, and the bright C-H of poor stave of its infrared spectrum is at 2850cm -1~ 3000cm -1between have obvious absorption peak; C-H2# gas powder C and Si percentage composition are respectively 0.150 and 0.288, and the bright C-H of poor stave of its infrared spectrum is at 2850cm equally -1~ 3000cm -1between have obvious absorption peak.
As can be seen from the present embodiment data, infrared spectrum difference spectrum identical, the change of C is identical, the change of Si is also identical, so just think titanium dioxide surface organic process time C and Si be all stable, thus judge titanium dioxide surface organic process be stable.
Evaluation method provided by the invention has good application and promotion prospect in organic surface treatment of the inorganic pigments such as titanium dioxide and filler.

Claims (6)

1. detect a method for titanium dioxide surface organic process stability, it is characterized in that: comprise the following steps:
A, more than one batch three is washed material and wash by every batch three and expect that the gas powder of more than two batches prepared is dried respectively to constant weight;
B, with infrared spectrometer detect respectively dry to three of constant weight wash material gentle powder, obtain respective infrared spectrogram respectively;
C, to compare according to above-mentioned infrared spectrogram, obtain the poor spectrogram that a certain batch three is washed material and every batch of gas powder prepared therefrom; If it is variant that these differences compose characteristic peak positions each other, then think that titanium dioxide surface organic process is unstable; If these differences compose characteristic peak positions each other do not have difference, then carry out steps d;
Or compare according to above-mentioned infrared spectrogram, obtain a certain batch three and wash material and the poor spectrogram of every batch of gas powder prepared therefrom and another batch three and wash and expect and the poor spectrogram of every batch of gas powder prepared therefrom; If it is variant that these differences compose characteristic peak positions each other, then think that titanium dioxide surface organic process is unstable; If these differences compose characteristic peak positions each other do not have difference, then carry out steps d;
D, by organic agent dry to constant weight, with its whole element of energy spectrometer qualitative detection;
E, the element contained by organic agent recorded according to steps d, more quantitatively detect respectively dry to three of constant weight wash in the gentle powder of material to the corresponding element contained by organic agent;
F, data analysis according to step e, outside removing metrical error, obtain a certain batch three and wash material and each constituent content difference in every batch of gas powder prepared therefrom; If each constituent content difference is all identical, then think that titanium dioxide surface organic process is stablized; If there is a constituent content difference different, then think that titanium dioxide surface organic process is unstable;
Or according to the data analysis of step e, outside removing error-detecting, obtain a certain batch and to wash with each constituent content difference and another batch three in gas powder prepared therefrom and expect and each constituent content difference in gas powder prepared therefrom; If each constituent content difference is all identical, then think that titanium dioxide surface organic process is stablized; If there is a constituent content difference different, then think that titanium dioxide surface organic process is unstable.
2. the method for detection titanium dioxide surface according to claim 1 organic process stability, is characterized in that: comprise the following steps:
A, a certain for titanium dioxide batch three is washed material and washed by this batch three and expect that the gas powder of more than two batches prepared is dried respectively to constant weight;
B, with infrared spectrometer detect respectively dry to three of constant weight wash material gentle powder, obtain respective infrared spectrogram respectively;
C, to compare according to above-mentioned infrared spectrogram, obtain the poor spectrogram that this batch three washes material and every batch of gas powder prepared therefrom; If it is variant that these differences compose characteristic peak positions each other, then think that titanium dioxide surface organic process is unstable; If these differences compose characteristic peak positions each other do not have difference, then carry out steps d;
D, by organic agent dry to constant weight, with its whole element of energy spectrometer qualitative detection;
E, the element contained by organic agent recorded according to steps d, more quantitatively detect respectively dry to three of constant weight wash in the gentle powder of material to the corresponding element contained by organic agent;
F, data analysis according to step e, outside removing metrical error, obtain this batch three and wash each constituent content difference in material and every batch of gas powder prepared therefrom; If each constituent content difference is all identical, then think that titanium dioxide surface organic process is stablized; If there is a constituent content difference different, then think that titanium dioxide surface organic process is unstable.
3. the method for detection titanium dioxide surface according to claim 1 and 2 organic process stability, it is characterized in that: in step a, described bake out temperature is 105 ~ 120 DEG C, and the time is 24 ~ 36h.
4. in the method step b of detection titanium dioxide according to claim 1 and 2 surface organic process stability, Dai test sample Pin ︰ potassium bromide=1 ︰ 20 ~ 25 in mass ratio during infrared spectrometer compressing tablet.
5., in the method step d of detection titanium dioxide according to claim 1 and 2 surface organic process stability, described bake out temperature is 105 ~ 110 DEG C, and the time is 4 ~ 8h.
6., in the method step e of detection titanium dioxide according to claim 1 and 2 surface organic process stability, described quantitative detection is 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
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