CN113816389A - Method for synthesizing high-purity hemimorphite by hydrothermal method - Google Patents
Method for synthesizing high-purity hemimorphite by hydrothermal method Download PDFInfo
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- CN113816389A CN113816389A CN202111234063.XA CN202111234063A CN113816389A CN 113816389 A CN113816389 A CN 113816389A CN 202111234063 A CN202111234063 A CN 202111234063A CN 113816389 A CN113816389 A CN 113816389A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/45—Aggregated particles or particles with an intergrown morphology
Abstract
The invention belongs to the technical field of artificial synthesis of natural minerals, and particularly relates to a synthetic method of high-purity hemimorphite. The method takes chemically pure zinc metasilicate as a raw material, the zinc metasilicate is weighed according to the liquid-solid ratio of 8-16mL/g, the zinc metasilicate is placed into a reaction kettle, distilled water with the corresponding ratio is added into the kettle, and the reaction is continued for 1-4 hours under the conditions of the rotation speed of 800rpm at 200-. The mineral prepared by the synthetic method of the invention is analyzed by X-ray diffraction, and the characteristic peak of hemimorphite is found to be very obvious and high in peak intensity in the X-ray diffraction pattern, while the characteristic peak of the non-aluminum-zinc saponite and the raw material zinc metasilicate is very weak and not very obvious. Therefore, the hemimorphite synthesized by the method has high purity, good crystal form, simple reaction, easy operation and convenient production and preparation, can provide raw materials for researching relevant properties of the hemimorphite, can also be used for simulating the relevant experimental tests of thermodynamics and the like when natural minerals and chemical reagents interact, and solves the technical problems of complex process, long reaction time, low purity of obtained samples and the like of the conventional hemimorphite preparation method.
Description
Technical Field
The invention belongs to the technical field of artificial synthesis of natural minerals, and particularly relates to a method for synthesizing high-purity hemimorphite by a hydrothermal method.
Background
Hemimorphite (hemimorphite) is an important mineral resource and has the chemical formula: zn4Si2O7(OH)2·H2And O. The hemimorphic ore has an important economic status in the zinc smelting industry, and because the hemimorphic ore belongs to silicate minerals and has a complex internal structure, the surface structure of the minerals is uneven, the minerals are easy to argillization and difficult to sort, and the quantity of pure hemimorphic ores which can be used for research is less, and the research of related chemical theories is difficult to carry out, so that a large quantity of hemimorphic ores can not be effectively utilized. The zinc silicate inorganic mineral is an ideal base material, has an energy gap of 5.5eV, an exciton confinement energy of 75meV and good light transmission in an ultraviolet and visible region, and is widely applied to the fields of coatings, corrosion protection of steel, cathode ray tubes, up-conversion luminescent materials, catalysts and the like. However, the hemimorphite zinc silicate in the nature has low purity and is difficult to separate and extract, the existing synthesis technology has complex reaction, strict control requirement on the amount of reactants and lower purity, and the requirements of related scientific and technological fields are difficult to meet.
Therefore, improvement to these disadvantages is needed to search for a new synthetic method of high-purity hemimorphite.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the artificial synthesis method of the high-purity hemimorphite, and the hemimorphite synthesized by the method has the advantages of good crystal form, high purity, simple reaction and easy control, and can meet the requirements of various industries.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a method for synthesizing high-purity hemimorphite by a hydrothermal method takes chemically pure zinc metasilicate as a raw material, and the high-purity hemimorphite is prepared by the hydrothermal synthesis method, and the method comprises the following specific steps:
(1) weighing zinc metasilicate according to the liquid-solid ratio of 8-16mL/g, placing the zinc metasilicate into a reaction kettle, adding distilled water with a corresponding proportion into the reaction kettle, and carrying out hydrothermal reaction for 1-4 hours at the rotating speed of 800rpm, the pressure of 0.4-1.2MPa and the temperature of 240 ℃ under 200-;
(2) carrying out liquid-solid separation on the substances obtained by the reaction, and then drying for 6-12 hours at the temperature of 50-80 ℃ to obtain the high-purity hemimorphite Zn4Si2O7(OH)2·H2O。
The liquid-solid ratio in the step (1) is 8-16 mL/g.
The reaction kettle in the step (1) is a closed pressure reaction kettle with a mechanical stirring device.
In the step (1), the distilled water is secondary distilled water.
The rotation speed in the step (1) of the invention is 200-800 rpm.
The pressure in the step (1) is 0.4-1.2 MPa.
The hydrothermal reaction temperature in the step (1) of the present invention is preferably controlled at 220 ℃.
The hydrothermal reaction time in the step (1) of the invention is 1-4 hours.
The liquid-solid separation tool in the step (2) is a vacuum pump.
In the step (2), the drying temperature of the sample is 50-80 ℃, the drying time is 6-12 hours, and the drying tool is an air blowing drying oven.
The invention has the beneficial effects that: the zinc metasilicate is weighed according to a certain liquid-solid ratio and is put into a reaction kettle, the artificial synthesis of the high-purity hemimorphite is realized under certain hydrothermal reaction conditions, the reaction conditions are mild, the reaction is simple, the operation is easy, the large-scale production is convenient, and the high-purity hemimorphite can be prepared by using the synthesis method disclosed by the invention, does not contain other impurities, and is convenient to apply to the scientific and technological field with high requirements.
Drawings
FIG. 1 is an XRD powder diffraction pattern of samples obtained at different temperatures;
FIG. 2 is a XRD powder diffraction pattern of samples obtained at different reaction times at 200 ℃;
FIG. 3 is a XRD powder diffraction pattern of samples obtained at different reaction times at 220 ℃;
FIG. 4 is a XRD powder diffraction pattern of samples obtained at different charge levels of zinc metasilicate at 220 ℃;
FIG. 5 is an SEM image of a sample obtained at 220 ℃ under conditions of a liquid-solid ratio of 12mL/g, a reaction time of 3 hours, a rotation speed of 600rpm, a pressure of 1.0 MPa.
Detailed Description
The following examples are intended to further illustrate the invention, but are not intended to limit the invention.
Example 1
Weighing 50g of zinc metasilicate according to the liquid-solid ratio of 12mL/g, placing the zinc metasilicate into a 1L reaction kettle, adding 600mL of distilled water into the kettle, sealing the reaction kettle, introducing industrial oxygen, respectively setting the temperature to be 140-220 ℃ at the constant rotating speed of 600rpm and the pressure of 1.0MPa, starting timing when the temperature is raised to the set temperature, and carrying out hydrothermal reaction for 3 hours at the temperature; cooling to 70 ℃ through a water cooling pipe, carrying out liquid-solid separation on the substances obtained by the reaction, and then drying for 10 hours at the temperature of 65 ℃.
Figure 1 is an XRD powder diffractogram of the resulting samples at different temperatures. As can be seen from FIG. 1, when the reaction temperature is lower than 200 ℃, the XRD pattern of the obtained sample has no obvious change along with the increase of the reaction temperature and is basically consistent with the XRD pattern of the raw material zinc metasilicate; when the reaction temperature is increased to 200 ℃, the characteristic peak of the zinc metasilicate almost completely disappears, and the phases detected by XRD are mainly hemimorphite and trace aluminum-free sauconite; after the temperature is continuously raised to 220 ℃, the obtained sample is heteropolar ore, and has good crystal form and high purity. It is considered that the temperature for synthesizing high-purity hemimorphite should be 200 ℃ and above.
Example 2
Weighing 50g of zinc metasilicate according to the liquid-solid ratio of 12mL/g, putting the zinc metasilicate into a 1L reaction kettle, adding 600mL of distilled water into the kettle, sealing the reaction kettle, introducing industrial oxygen, starting timing when the temperature is raised to 200 ℃ at the constant rotating speed of 600rpm and the pressure of 1.0MPa, and respectively setting the hydrothermal reaction for 1-3 hours at the temperature; cooling to 70 ℃ through a water cooling pipe, carrying out liquid-solid separation on the substances obtained by the reaction, and then drying for 10 hours at the temperature of 65 ℃.
FIG. 2 is a XRD powder diffraction pattern of samples obtained at different reaction times at 200 ℃. As can be seen from FIG. 2, when the hydrothermal reaction temperature is 200 ℃, the XRD pattern of the synthesized product has no obvious change in the process of prolonging the reaction time to 2 hours, and is basically consistent with the XRD pattern of the raw material zinc metasilicate; the reaction time is continuously prolonged to 2.5h, and the main phases in the obtained sample are heteropolar ore, a small amount of aluminum-free zinc saponite and trace zinc metasilicate; when the hydrothermal reaction time is 3 hours, the phases detected by XRD are mainly hemimorphite and trace aluminum-free sauconite, and the characteristic peak of zinc metasilicate almost completely disappears, so that the temperature for synthesizing high-purity hemimorphite at 200 ℃ is considered to be more than 3 hours.
Example 3
Weighing 50g of zinc metasilicate according to the liquid-solid ratio of 12mL/g, putting the zinc metasilicate into a 1L reaction kettle, adding 600mL of distilled water into the kettle, sealing the reaction kettle, introducing industrial oxygen, starting timing when the temperature is raised to 220 ℃ at the constant rotating speed of 600rpm and the pressure of 1.0MPa, and respectively setting the hydrothermal reaction for 1-3 hours at the temperature; cooling to 70 ℃ through a water cooling pipe, carrying out liquid-solid separation on the substances obtained by the reaction, and then drying for 10 hours at the temperature of 65 ℃.
FIG. 3 is a XRD powder diffraction pattern of samples obtained at different reaction times at 220 ℃. As can be seen from FIG. 3, under the condition that the hydrothermal reaction temperature is 220 ℃, the XRD pattern of the obtained sample has no obvious change along with the prolonging of the reaction time to 1h, and is basically consistent with the XRD pattern of the raw material zinc metasilicate; when the reaction time is 1.5h, the main phases of the obtained sample are heteropolar ore, a small amount of zinc metasilicate and trace aluminum-free soapstone; the reaction time is continuously prolonged to 3h, XRD results show that the characteristic peak of the aluminum-free zinc saponite disappears after being enhanced, the characteristic peak of the zinc metasilicate almost completely disappears, the obtained sample is heteropolar, the crystal form is good, the purity is high, and the fact that the hydrothermal reaction time is prolonged at 220 ℃ is also beneficial to synthesizing high-purity heteropolar. Therefore, it is considered that the synthesis of high purity hemimorphite is facilitated by increasing the reaction temperature and extending the reaction time.
Example 4
Respectively weighing 50g and 150g of zinc metasilicate according to the liquid-solid ratio of 12mL/g, respectively placing the zinc metasilicate into a 1L reaction kettle and a 3L reaction kettle, respectively adding 0.6L distilled water and 1.8L distilled water into the kettles, sealing the reaction kettles, introducing industrial oxygen, and carrying out hydrothermal reaction for 3 hours at the rotating speed of 600rpm, the pressure of 1.0MPa and the temperature of 220 ℃; cooling to 70 ℃ through a water cooling pipe, carrying out liquid-solid separation on the substances obtained by the reaction, and then drying for 10 hours at the temperature of 65 ℃.
FIG. 4 is a XRD powder diffraction pattern of samples obtained with different charge amounts of zinc metasilicate at 220 ℃. As can be seen from FIG. 4, with the increase of the charging amount of the raw material zinc metasilicate, the XRD patterns of the samples obtained under the charging amount of 1 time and the charging amount of 3 times have no obvious difference, the main phase is heteropolar, and the heteropolar mineral has good crystal form and high purity. Therefore, the method considers that the same-proportion amplification of the zinc metasilicate feeding amount has no obvious influence on the obtained sample, and can provide certain technical support for large-scale preparation of the hemimorphite.
Example 5
Weighing 50g of zinc metasilicate according to the liquid-solid ratio of 12mL/g, putting the zinc metasilicate into a 1L reaction kettle, adding 600mL of distilled water into the kettle, sealing the reaction kettle, introducing industrial oxygen, and carrying out hydrothermal reaction for 3 hours at the rotating speed of 600rpm, the pressure of 1.0MPa and the temperature of 220 ℃; and cooling to 70 ℃ through a water cooling pipe, carrying out liquid-solid separation on the substances obtained by the reaction, and drying for 10 hours at the temperature of 65 ℃ to obtain a sample, namely the high-purity hemimorphite.
FIG. 5 is an SEM image of a sample obtained under preferred conditions. As can be seen from the SEM image, the morphology of the heteropolar ore is a petaloid structure stacked in a rod shape, no other morphology appears, and the heteropolar ore is proved to be high-purity heteropolar ore.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that several changes and modifications may be made without departing from the spirit and scope of the invention, which should not be construed as affecting the effectiveness of the invention and its patentability. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (4)
1. A method for synthesizing high-purity hemimorphite by a hydrothermal method is characterized by comprising the following steps:
(1) taking chemically pure zinc metasilicate as a raw material, weighing the zinc metasilicate according to the liquid-solid ratio of 8-16mL/g, putting the zinc metasilicate into a reaction kettle, adding distilled water with a corresponding ratio into the kettle, and carrying out hydrothermal reaction for 3-4 hours under the conditions of 200-800rpm rotation speed, 0.4-1.2MPa pressure and 220 ℃;
(2) and (3) carrying out liquid-solid separation on the substances obtained by the reaction, and then drying for 6-12 hours at the temperature of 50-80 ℃ to obtain a sample, namely the high-purity hemimorphite.
2. The hydrothermal synthesis of highly pure hemimorphite according to claim 1, wherein: the starting material is chemically pure zinc metasilicate.
3. The hydrothermal synthesis of highly pure hemimorphite according to claim 1, wherein: the reaction kettle is a closed pressure reaction kettle with a mechanical stirring device.
4. The hydrothermal synthesis of highly pure hemimorphite according to claim 1, wherein: in the hydrothermal reaction process, the temperature in the reaction kettle is 180-240 ℃, and the hydrothermal reaction time is 1-4 hours.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1050510A1 (en) * | 1997-06-23 | 2000-11-08 | Basf Aktiengesellschaft | Process for the preparation of a hemimorphite catalyst |
| CN106145691A (en) * | 2016-07-06 | 2016-11-23 | 昆明理工大学 | A kind of method of the smithsonite zinc silicate of direct growth on a glass substrate |
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- 2021-10-22 CN CN202111234063.XA patent/CN113816389A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1050510A1 (en) * | 1997-06-23 | 2000-11-08 | Basf Aktiengesellschaft | Process for the preparation of a hemimorphite catalyst |
| CN106145691A (en) * | 2016-07-06 | 2016-11-23 | 昆明理工大学 | A kind of method of the smithsonite zinc silicate of direct growth on a glass substrate |
Non-Patent Citations (1)
| Title |
|---|
| 李均培 等: "水热法合成异极矿的研究", 《科技创新导报》 * |
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