CN113252418A - Preparation method of sulfuric acid method titanium dioxide acidolysis solid-phase substance polished sample - Google Patents
Preparation method of sulfuric acid method titanium dioxide acidolysis solid-phase substance polished sample Download PDFInfo
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- CN113252418A CN113252418A CN202110546290.XA CN202110546290A CN113252418A CN 113252418 A CN113252418 A CN 113252418A CN 202110546290 A CN202110546290 A CN 202110546290A CN 113252418 A CN113252418 A CN 113252418A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/36—Embedding or analogous mounting of samples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/36—Embedding or analogous mounting of samples
- G01N2001/366—Moulds; Demoulding
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Abstract
The invention provides a preparation method of a sulfate process titanium dioxide acidolysis solid-phase substance polished sample, which comprises the following steps: flatly paving the sulfuric acid process titanium dioxide acidolysis solid-phase powder at the bottom of a sample groove of a hot-setting machine, adding a setting material to uniformly cover the surface of the sulfuric acid process titanium dioxide acidolysis solid-phase powder, and starting the hot-setting machine to set a sample to obtain a setting sample; grinding the embedded sample to obtain a ground sample; and polishing the ground sample to obtain a sulfuric acid process titanium dioxide acidolysis solid-phase substance polished sample. The method provided by the invention can effectively solve the problem that the traditional cold-inlaid resin cannot effectively solidify the acidolysis solid-phase substance with stronger acidity, has high solidification strength, compact interior and surface of the solidified sample and no air holes, ensures that the solidified acidolysis solid-phase sample is not easy to fall off, and can be visually used for large-scale equipment such as an electron microscope, a mineral analyzer, an energy spectrometer and the like by a polished acidolysis solid-phase substance polished sheet to research the composition, morphology, components and other characteristics of all phases in the sulfuric acid method titanium dioxide acidolysis stage.
Description
Technical Field
The invention belongs to the technical field of sample preparation, and particularly relates to a preparation method of a sulfuric acid method titanium dioxide acidolysis solid-phase substance polished sample.
Background
The sulfate process of titanium dioxide is one of two major titanium dioxide production processes in the world at present, and is widely applied to various countries in the world due to the universality of the titanium-containing raw materials, in particular to developing countries with limited technology. The acidolysis process is a key technical link of titanium white production by a sulfuric acid method, and the definition of the acidolysis process mechanism has great significance for improving the acidolysis process and further improving the titanium white productivity and quality. For a long time, most of analysis on the phase of the titanium dioxide acidolysis solid phase substance by the sulfuric acid method is to analyze residues after hydrolysis, namely, the mechanism of the acidolysis process is reversely deduced by analyzing the phase composition, content and shape change of the residues at different periods of acidolysis. The sulfuric acid method titanium dioxide production adopts concentrated sulfuric acid to perform titanium ore acidolysis, so that acidolysis solid-phase substances are very strong in acidity, a curing agent ethylenediamine needs to be added to cure a sample when epoxy resin is used for preparing an optical sheet sample which can be used by a power supply mirror, the ethylenediamine is an alkaline substance and can react with an acidic substance in the acidolysis solid-phase substances, so that epoxy resin is poor in consolidation, optical sheet preparation fails, and subsequent phase analysis cannot be carried out.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing a sulfate process titanium dioxide acidolysis solid-phase substance polished sample, which can obtain a sulfate process titanium dioxide acidolysis solid-phase substance polished sample with good quality.
The invention provides a preparation method of a sulfate process titanium dioxide acidolysis solid-phase substance polished sample, which comprises the following steps:
flatly paving the sulfuric acid process titanium dioxide acidolysis solid-phase powder at the bottom of a sample groove of a hot-setting machine, adding a setting material to uniformly cover the surface of the sulfuric acid process titanium dioxide acidolysis solid-phase powder, and starting the hot-setting machine to set a sample to obtain a setting sample;
grinding the embedded sample to obtain a ground sample;
and polishing the ground sample to obtain a sulfuric acid process titanium dioxide acidolysis solid-phase substance polished sample.
Preferably, the granularity of the sulfuric acid method titanium dioxide acidolysis solid-phase material powder is 300-350 meshes.
Preferably, the inlays are hot melt gums.
Preferably, the ingredient of the hot melt gum is a phenolic resin.
Preferably, the mass ratio of the sulfuric acid method titanium dioxide acidolysis solid-phase material powder to the mosaic material is (2-3): 10.
preferably, the inlaying time of the sample is 10-20 min; the temperature is 140-160 ℃; the pressure is 140 to 160 bar.
Preferably, the grinding time is less than or equal to 1min by using 180-800-mesh sand paper in the grinding process; the time for grinding by using 1200-mesh sand paper is less than or equal to 1.5 min.
Preferably, the pressure of the grinding is 20-30N.
Preferably, the polishing paste used in the polishing process is an alumina polishing paste.
Preferably, the polishing time is 2-4 min.
The preparation method of the sulfuric acid process titanium dioxide acidolysis solid-phase substance polished sheet sample provided by the invention is simple to operate, can effectively solve the problem that the traditional cold-inlaid resin cannot effectively solidify the acidolysis solid-phase substance with stronger acidity, has high solidification strength, is compact in the interior and surface of the solidified sample, has no air holes, is not easy to fall off from the solidified acidolysis solid-phase substance sample, and can be directly used for large-scale equipment such as an electron microscope, a mineral analyzer and an energy spectrometer to study the composition, morphology, components and other characteristics of all phases in the sulfuric acid process titanium dioxide acidolysis stage.
Drawings
FIG. 1 is a photograph of a slide sample prepared in comparative example 1 of the present invention;
FIG. 2 is a photograph of a slide sample prepared in example 1 of the present invention;
FIG. 3 is a scanning electron microscope image of the polished section prepared in example 1 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other examples, which may be modified or appreciated by those of ordinary skill in the art based on the examples given herein, are intended to be within the scope of the present invention. It should be understood that the embodiments of the present invention are only for illustrating the technical effects of the present invention, and are not intended to limit the scope of the present invention. In the examples, the methods used were all conventional methods unless otherwise specified.
The invention provides a preparation method of a sulfate process titanium dioxide acidolysis solid-phase substance polished sample, which comprises the following steps:
flatly paving the sulfuric acid process titanium dioxide acidolysis solid-phase powder at the bottom of a sample groove of a hot-setting machine, adding a setting material to uniformly cover the surface of the sulfuric acid process titanium dioxide acidolysis solid-phase powder, and starting the hot-setting machine to set a sample to obtain a setting sample;
grinding the embedded sample to obtain a ground sample;
and polishing the ground sample to obtain a sulfuric acid process titanium dioxide acidolysis solid-phase substance polished sample.
In the present invention, the method for producing the sulfate process titanium dioxide acidolysis solid-phase material powder preferably includes:
mixing concentrated sulfuric acid and titanium ore powder to obtain a mixture;
carrying out acidolysis reaction on the mixture and water to obtain a reaction product;
and heating the reaction product, and curing to obtain sulfuric acid process titanium dioxide acidolysis solid-phase substance powder.
In the invention, the mass fraction of the concentrated sulfuric acid is preferably 95-99%, more preferably 96-98%, more preferably 97-98%, and most preferably 98%.
In the invention, the granularity of the titanium ore powder is preferably 300-350 meshes, more preferably 310-340 meshes, more preferably 320-330 meshes, and most preferably 325 meshes.
In the invention, the mass ratio of the concentrated sulfuric acid to the titanium ore powder is preferably (1.5-2): 1, more preferably (1.6 to 1.8): 1, most preferably 1.7: 1.
in the present invention, the mixing is preferably performed under stirring; the stirring time is preferably 3-7 min, more preferably 4-6 min, and most preferably 5 min.
In the invention, the mass ratio of the titanium ore powder to water is preferably (4-5): 1, more preferably (4.2 to 4.8): 1, more preferably (4.4 to 4.6): 1, most preferably 4.5: 1.
in the invention, the heating temperature is preferably 120-140 ℃, more preferably 125-135 ℃, and most preferably 130 ℃.
In the invention, after the heating is finished, the temperature of the heated reaction system is preferably reduced and then the reaction system is cured; the curing temperature is preferably 160-200 ℃, more preferably 170-190 ℃, and most preferably 180 ℃; the maturation is preferably carried out in a forced air drying oven; the curing time is preferably 0.5 to 1.5 hours, more preferably 0.8 to 1.2 hours, and most preferably 1 hour.
In the invention, the granularity of the sulfuric acid method titanium dioxide acidolysis solid-phase material powder is preferably 300-350 meshes, more preferably 310-340 meshes, more preferably 320-330 meshes, and most preferably 325 meshes.
In the present invention, the ingredient of the inlay, preferably a hot melt gum, is preferably phenolic resin powder.
In the invention, the mass ratio of the sulfuric acid method titanium dioxide acidolysis solid-phase material powder to the mosaic material is preferably (2-3): 10, more preferably (2.2 to 2.8): 10, more preferably (2.4 to 2.6): 10, most preferably 2.5: 10.
in the present invention, before starting the hot inlaying machine to inlay the sample, the method preferably further includes:
putting the pressing block, closing the pressing bolt and screwing.
In the invention, the time in the sample inlaying process is preferably 10-20 min, more preferably 12-18 min, more preferably 14-16 min, and most preferably 15 min; the temperature in the sample inlaying process is preferably 140-160 ℃, more preferably 145-155 ℃, and most preferably 150 ℃; the pressure in the sample inlaying process is preferably 140-160 bar, more preferably 145-155 bar, and most preferably 150 bar.
In the invention, the grinding is preferably performed by a semi-automatic grinding and polishing machine; the specification of the sand paper used for grinding is preferably 180 meshes, 400 meshes, 800 meshes and 1200 meshes; the using sequence of the sand paper in the grinding process is preferably gradually changed from coarse to fine, namely from 180-mesh sand paper to 1200-mesh sand paper. In the invention, the grinding time of the 180-800-mesh sand paper in the grinding process is preferably less than or equal to 1min, more preferably 0.5-1 min, more preferably 0.6-0.9 min, and most preferably 0.7-0.8 min; the grinding time of the 1200-mesh sand paper in the grinding process is preferably less than or equal to 1.5min, more preferably 1-1.5 min, more preferably 1.1-1.4 min, and most preferably 1.2-1.3 min; the pressure in the grinding process is preferably 20-30N, more preferably 22-28N, more preferably 24-26N, and most preferably 25N; the grinding method is preferably dry grinding, namely, no water is added in the grinding process.
In the invention, the polishing is preferably performed by manually polishing with black long-pile polishing cloth; the polishing paste adopted in the polishing process is preferably aluminum oxide polishing paste, and the particle size of the polishing paste is preferably 2-3 micrometers, more preferably 2.2-2.8 micrometers, more preferably 2.4-2.6 micrometers, and most preferably 2.5 micrometers; preferably, no water is added during the polishing process; in the polishing process, the samples are preferably rotated at small angles of 15-25 s to ensure the polishing effect, more preferably 18-22 s, and most preferably 20 s; the angle of the small-angle rotation is preferably 5-15 degrees, more preferably 8-12 degrees, and most preferably 10 degrees; the time in the polishing process is preferably 2-4 min, more preferably 2.5-3.5 min, and most preferably 3 min.
In the present invention, it is preferable that the polishing further comprises:
and wiping off residual polishing paste, fluff and other stains on the surface of the polished sample by using a piece of lens wiping paper so as to ensure that the surface of the sample is bright.
In the present invention, after obtaining the sulfate process titanium dioxide acidolysis solid-phase substance polished sample, the method preferably further comprises:
and (5) checking whether the polished section sample is qualified.
In the present invention, the method of checking preferably includes:
and (3) placing the sulfuric acid method titanium dioxide acidolysis solid-phase polished section sample under an optical microscope for observation, confirming whether scratches exist on the surface of the polished section sample, and whether the mineral boundary and the mineral surface are clear, and repeating the grinding and polishing operations until the polished section sample meets the requirements if the scratches exist on the surface of the polished section sample or the mineral boundary and the surface are not clear.
The preparation method of the sulfuric acid process titanium dioxide acidolysis solid-phase substance polished sheet sample provided by the invention is simple to operate, can effectively solve the problem that the traditional cold-inlaid resin cannot effectively solidify the acidolysis solid-phase substance with stronger acidity, has high solidification strength, is compact in the interior and surface of the solidified sample, has no air holes, is not easy to fall off from the solidified acidolysis solid-phase substance sample, and can be directly used for large-scale equipment such as an electron microscope, a mineral analyzer and an energy spectrometer to study the composition, morphology, components and other characteristics of all phases in the sulfuric acid process titanium dioxide acidolysis stage.
The titanium dioxide acidolysis solid-phase substance powder adopted in the embodiment of the invention is prepared by the following method: mixing the raw materials in a ratio of 1.7: respectively weighing a certain amount of concentrated sulfuric acid (mass fraction is 98%) and titanium ore powder (particle size is 325 meshes) according to the acid ore ratio of 1, then sequentially adding the concentrated sulfuric acid and the titanium ore powder into a 1L beaker, uniformly stirring for 5min, weighing a proper amount of water (the mass ratio of the water to the titanium ore powder is 1: 4.5) and adding the water into the beaker to initiate acidolysis reaction, then placing the beaker into an electric heating jacket, heating to 130 ℃ and stopping, taking out the beaker, placing the beaker into a forced air drying oven to age for 1h at 180 ℃ after the temperature of a reaction system is reduced, and then taking out a sample in the beaker to obtain the sulfuric acid process titanium dioxide acidolysis solid-phase substance powder.
The hot setting machine adopted in the embodiment of the invention is equipment of the Standard music Simplimet 1000 type, and the hot melt gum is the Standard music PhenocureTMThe type of product, alumina polishing paste, is a W2.5 product provided by Guiyang sixth grinding wheel factory.
Comparative example 1
Epoxy resin (type: Epoxicure) is adoptedTM2, manufacturer: biaole) and ethylenediamine curing agent inlaid sulfuric acid method titanium dioxide acidolysis solid-phase sample, and the specific method comprises the following steps:
taking 3g of sulfuric acid process titanium dioxide acidolysis solid-phase powder, paving the powder at the bottom of a mold with the inner diameter of 3cm, then sequentially adding 6g of epoxy resin and 1.5g of ethylenediamine curing agent according to the proportion of 4:1, uniformly stirring until no bubbles are generated, then putting the mold into a vacuum kettle, starting a motor to pump out air in the kettle, stopping the motor when the vacuum degree in the kettle is-25 to-20 kPa, and standing for 6-8 hours.
The picture of the sulfuric acid process titanium dioxide acidolysis solid-phase polished sample prepared in comparative example 1 of the invention is shown in fig. 1, and as can be seen from fig. 1, the sample is poor in consolidation, the sample surface is soft, and a large number of holes are formed on the surface and inside of the sample.
Example 1
Taking 3g of dried titanium dioxide acidolysis solid-phase powder by a sulfuric acid method, uniformly paving the powder on the surface of a sample tank of a hot embedding machine, adding a spoon (about 10g) of an embedding material (hot-melt gum) to uniformly cover the surface of the sample, then putting a pressing block, closing a pressing bolt and screwing down; and starting the hot inlaying machine to begin inlaying the sample, wherein the time is set to be 15min, the temperature is 130 ℃, and the pressure is 150 bar.
Polishing a polished section: grinding the sample by using a semi-automatic grinding and polishing machine, wherein the specification of sand paper is 180 meshes, 400 meshes, 800 meshes and 1200 meshes, the grinding sequence is gradually transited from 180 meshes to 1200 meshes from coarse to fine, and the grinding time is set as: 180-800 meshes to 1min (180 meshes: 1min, 400 meshes: 1min, 800 meshes: 1min), 1200 meshes to 1.5min (1-1.5 min), and the grinding pressure is set to 25N; the grinding process is dry grinding without adding water.
Polishing an optical sheet: and (3) manually polishing the ground sample by using black long-velvet polishing cloth, selecting 2.5-micron-size alumina polishing paste, adding no water in the polishing process, rotating the sample at small angles (10 degrees) of about 20s to ensure the polishing effect of the sample, and polishing for about 3 min. The special lens wiping paper is used for carefully wiping off stains such as polishing paste, fluff and the like remained on the surface of the polished sample so as to ensure that the surface of the sample is bright.
And (3) checking whether the polished section is qualified: and (3) placing the prepared polished section under an optical microscope for observation, confirming whether the surface of the sample has scratches or whether the mineral boundary and the mineral surface are clear, and repeating the grinding and polishing steps if the surface of the sample has scratches or the mineral boundary and the mineral surface are not clear until the sample meets the requirements.
The picture of the polished section sample prepared in the embodiment 1 of the invention is shown in fig. 2, and as can be seen from fig. 2, the sample is compact, has no pores and has good consolidation, and various phases corresponding to the acidolysis process can be observed in the polished section sample, including key products of titanyl sulfate and the like.
The optical sheet sample prepared in the embodiment 1 of the invention is gilded (the optical sheet sample is gilded by a vacuum ion sputtering coating instrument, the polished surface of the sample is placed on a sample seat in a machine upwards, then a top cover of the machine is closed, a gilding mode is started, and the sample is taken out after the process is finished (the time is about 15 min)), the appearance of the phase of the sample is detected and observed by a scanning electron microscope, the detection result is shown in figure 3, and the appearance of each phase in an acidolysis solid phase substance under the electron microscope is visual and clear, so that the method can be effectively applied to the mechanism research of the acidolysis process.
The preparation method of the sulfuric acid process titanium dioxide acidolysis solid-phase substance polished sheet sample provided by the invention is simple to operate, can effectively solve the problem that the traditional cold-inlaid resin cannot effectively solidify the acidolysis solid-phase substance with stronger acidity, has high solidification strength, is compact in the interior and surface of the solidified sample, has no air holes, is not easy to fall off from the solidified acidolysis solid-phase substance sample, and can be directly used for large-scale equipment such as an electron microscope, a mineral analyzer and an energy spectrometer to study the composition, morphology, components and other characteristics of all phases in the sulfuric acid process titanium dioxide acidolysis stage.
While only the preferred embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.
Claims (10)
1. A method for preparing a sulfate process titanium dioxide acidolysis solid-phase substance polished section sample comprises the following steps:
flatly paving the sulfuric acid process titanium dioxide acidolysis solid-phase powder at the bottom of a sample groove of a hot-setting machine, adding a setting material to uniformly cover the surface of the sulfuric acid process titanium dioxide acidolysis solid-phase powder, and starting the hot-setting machine to set a sample to obtain a setting sample;
grinding the embedded sample to obtain a ground sample;
and polishing the ground sample to obtain a sulfuric acid process titanium dioxide acidolysis solid-phase substance polished sample.
2. The method as claimed in claim 1, wherein the particle size of the sulfuric acid process titanium dioxide acidolysis solid-phase powder is 300-350 mesh.
3. The method of claim 1 wherein the inlays are hot melt gums.
4. The method of claim 1 wherein the hot melt gum is a phenolic resin.
5. The method as claimed in claim 1, wherein the mass ratio of the sulfuric acid method titanium dioxide acidolysis solid-phase material powder to the mosaic material is (2-3): 10.
6. the method according to claim 1, wherein the sample is mounted for 10-20 min; the temperature is 140-160 ℃; the pressure is 140 to 160 bar.
7. The method according to claim 1, wherein the grinding process is carried out by using 180-800-mesh sand paper for less than or equal to 1 min; the time for grinding by using 1200-mesh sand paper is less than or equal to 1.5 min.
8. The method according to claim 1, wherein the pressure for milling is 20-30N.
9. The method of claim 1, wherein the polishing paste used in the polishing process is an alumina polishing paste.
10. The method of claim 1, wherein the polishing time is 2-4 min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113740479A (en) * | 2021-08-18 | 2021-12-03 | 安徽迪诺环保新材料科技有限公司 | Method for qualitatively determining acidolysis rate degree of acid-ore mixture |
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Application publication date: 20210813 |