CN1284477A - Preparation and use of cerium tetrathiomolybdate - Google Patents
Preparation and use of cerium tetrathiomolybdate Download PDFInfo
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- CN1284477A CN1284477A CN 00122362 CN00122362A CN1284477A CN 1284477 A CN1284477 A CN 1284477A CN 00122362 CN00122362 CN 00122362 CN 00122362 A CN00122362 A CN 00122362A CN 1284477 A CN1284477 A CN 1284477A
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- tetrathiomolybdate
- cerium
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Abstract
The present invention synthesizes one kind of tetrathiomolybdate, especially cerium tetrathiomolybdate through a precipitation and conversion process. The compound has excellent tribological performance and may be used as solid lubricant for use at the temperature range from room temperature to 600 deg.C.
Description
The invention relates to thiomolybdate and a preparation method and application thereof.
The problem of high-temperature lubrication is an important research subject of tribology, and particularly, the development of a lubricant for realizing continuous lubrication from room temperature to high temperature is necessary. At present, most high-temperature solid lubricants have an initial lubricating temperature of more than 500 ℃, and most traditional solid lubricants are oxidized at about 300 ℃, so that the lubricants with continuous lubricating effect at room temperature to 500 ℃ are rare.
In the 70 s, ammonium thiomolybdate and cuprous ammonium thiomolybdate were used as drugs for treating liver diseases, but cadmium thiomolybdate was rarely involved. Especially, the application in high-temperature lubrication is less common.
The invention aims to provide tetrathiomolybdate.
Another object of the present invention is to provide a process for the preparation of tetrathiomolybdate.
It is a further object of the present invention to provide the use of tetrathiomolybdate.
A novel compound hasThe compound is found to be cerium thiomolybdate, and the specific compound is cerium tetrathiomolybdate with the molecular formula of Ce2(MoS4)3. The preparation method of the thiomolybdate adopts a precipitation conversion method, and the chemical reaction equation is as follows:
the specific method comprises the following steps:
taking CeCl3And Na2MoO4Respectively dissolving in water, adjusting pH =4-5, mixing the two compound solutions, keeping stirring for 1 hour, standing, aging, filtering, respectively washing with ammonium chloride aqueous solution with pH =5, water and diethyl ether, roasting at 500 ℃, taking out and crushing to obtain Ce2(MoO4)3。
Taking Ce prepared by the method2(MoO4)3Adding a small amount of water, dispersing for 30 minutes on an ultrasonic pulverizer, heating in a water bath to 60-70 ℃ after uniform dispersion, introducing pure hydrogen sulfide gas under stirring, performing suction filtration after complete conversion, washing, and drying to obtain the cerium tetrathiomolybdate.
The compound has good tribological performance and can be used as a solid lubricant at room temperature to 600 ℃. Meanwhile, the lubricating grease additive also has good tribological properties. The test method used was as follows:
2. friction test method
2.1 preparation of Friction test specimens
The friction test adopts a point contact mode, wherein an upper sample is α -Sialon (Sialon) ceramic balls with the diameter of 8mm, and a lower sample is W18Cr4V steel with the diameter of 19mm multiplied by 19mm, annular grooves with the inner diameter of 15mm and the outer diameter of 17mm and the depth of 0.07mm are carved on the friction surface of the lower sample, solid lubricant powder is firstly ground in an agate mortar and then put into acetone and dispersed in an ultrasonic crusher for 15 minutes, then a dropper is used for dropping the acetone solution onto the surface of the lower sample, and the lubricant powder is deposited on the surface of the annular grooves of the sample after the acetone is completely volatilized.
2.2 Friction test method the friction test was carried out using a ball-and-disc high-temperature friction tester. The loading load is 100N, the rotating speed is 300 r/min (the linear speed is 0.24 m/s), and the temperature is between room temperature and 600 ℃. In the test, a blank test when the pure ceramic ball and the steel are subjected to dry friction and a friction test when the pure ceramic ball and the steel are lubricated are carried out.
Example 1
Cerium tetrathiomolybdate (Ce)2(MoS4)3): get 4gCe2(MoO4)3Adding 25ml of deionized water, dispersing for 30 minutes on an ultrasonic pulverizer, heating in a water bath to 60-70 ℃ after uniform dispersion, introducing pure hydrogen sulfide gas for 8 hours under the condition of stirring, cooling after complete conversion, performing suction filtration, washing with deionized water, and drying at 105 ℃ to obtain the cerium tetrathiomolybdate. Taking out and crushing for later use.
The results of the friction test are shown in FIG. 1
FIG. 1 shows the presence of cerium tetrathiomolybdate (Ce)2(MoS4)3) Coefficient of friction versus temperature for powder lubricated and unlubricated conditions. It can be seen that in the blank experiment, the friction coefficient of the sialon ceramic ball and steel in the case of relative friction shows a higher friction coefficient (0.73) at 100 ℃, then decreases to a low value (0.36) at about 400 ℃, and then begins to increase again. In contrast, there is cerium tetrathiomolybdate (Ce)2(MoS4)3) Under the condition of powder lubrication, the friction coefficient of the lubricating oil is lower than that of a blank experiment in the whole test temperature range, and the friction coefficient change is small. The coefficient of friction reaches a low value (0.06) at 25 ℃ and then rises slowly, 0.11 at 200 ℃ and a maximum value (0.22) at 600 ℃.
Claims (3)
1. A tetrathiomolybdate characterised in that the compound is cerium tetrathiomolybdate.
2. A method for preparing cerium thiomolybdate, which is characterized by comprising the following steps: ce2(MoO4)3Adding a small amount of water, and performing ultrasonic treatmentDispersing for 30 minutes on a pulverizer, introducing pure hydrogen sulfide gas under the stirring condition after uniform dispersion, performing suction filtration after complete conversion, washing, and drying to obtain the tetrathio cerium aluminate.
3. A compound cerium tetrathiomolybdate is used as solid lubricant.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00122362 CN1284477A (en) | 2000-09-07 | 2000-09-07 | Preparation and use of cerium tetrathiomolybdate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00122362 CN1284477A (en) | 2000-09-07 | 2000-09-07 | Preparation and use of cerium tetrathiomolybdate |
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| Publication Number | Publication Date |
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| CN1284477A true CN1284477A (en) | 2001-02-21 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CN 00122362 Pending CN1284477A (en) | 2000-09-07 | 2000-09-07 | Preparation and use of cerium tetrathiomolybdate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101068749B (en) * | 2003-10-24 | 2010-09-01 | 英菲诺姆国际有限公司 | Process for producing ammonium polythiomolybdate of the formula (NH4)2Mo3S13.n H2O |
-
2000
- 2000-09-07 CN CN 00122362 patent/CN1284477A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101068749B (en) * | 2003-10-24 | 2010-09-01 | 英菲诺姆国际有限公司 | Process for producing ammonium polythiomolybdate of the formula (NH4)2Mo3S13.n H2O |
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