CN1095445C - Tetrathiomolybdate, and its preparing process and application - Google Patents
Tetrathiomolybdate, and its preparing process and application Download PDFInfo
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- CN1095445C CN1095445C CN99121024A CN99121024A CN1095445C CN 1095445 C CN1095445 C CN 1095445C CN 99121024 A CN99121024 A CN 99121024A CN 99121024 A CN99121024 A CN 99121024A CN 1095445 C CN1095445 C CN 1095445C
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- Prior art keywords
- tetrathio
- tetrathiomolybdate
- molybdate
- bacl
- methanol
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Abstract
The present invention discloses a tetrathiomolybdate, a preparation method thereof and an application thereof. The present invention synthesizes a novel tetrathiomolybdate, particularly compounds of zinc tetrathiomolybdenate and barium tetrathiomolybdenate. The present invention prepares the compounds by adopting an ionic reaction method. The compounds can be used as solid lubricant from the room temperature to 500 DEG C due to good tribological property.
Description
The present invention relates to a kind of tetrathiomolybdate and its production and use.
The high temperature lubricating problem is an important subject of tribology, especially develops a kind of lubricant and realizes from room temperature to high temperature following continuous lubrication necessity particularly.Its initial lubricated temperature of present most of high temperature solid lubricant is many more than 500 ℃, and the conventional solid lubricant is many oxidation has taken place when 300 ℃ of left and right sides, and the lubricant that therefore has the continuous lubrication effect between room temperature to 500 ℃ is more rare.
It is that medicine is used as the treatment hepatic diseases with sulfo-molybdenum acid ammonia and the cuprous ammonium of sulfo-molybdic acid that the people is arranged the seventies, but seldom relates to sulfo-zinc molybdate and sulfo-barium molybdate.Especially aspect high temperature lubricating, use just more rare.
The object of the present invention is to provide a kind of tetrathiomolybdate.
Another object of the present invention provides a kind of preparation method of tetrathiomolybdate.
Another purpose of the present invention provides the purposes of tetrathiomolybdate.
A kind of compound of novelty is found, and compound is a tetrathiomolybdate, and concrete compound is tetrathio zinc molybdate, tetrathio barium molybdate, and molecular formula is ZnMoS
4, BaMoS
4The preparation method of tetrathiomolybdate of the present invention adopts the method for ionic reaction, and concrete grammar is as follows:
Get equimolar Zn (Ac) respectively
22H
2O, BaCl
22H
2O and (NH
4)
2MoS
4Under nitrogen protection, be dissolved in the anhydrous methanol, treat that dissolving after-filtration fully removes impurity, under nitrogen, dropwise add Zn (Ac) again with the pulverizing of ultrasonic grinding machine
22H
2O, BaCl
22H
2The methanol solution of O, and keep stirring, wait to precipitate complete back and continue stirring and, isolate precipitation after the cooling in 50 ℃ of insulations 30 minutes, be product with oven dry after the methanol wash.
Compound involved in the present invention has good tribological property, can be used as solid lubricant and use under room temperature to 500 ℃.Adopt following test method to estimate:
2. rub(bing)test method
2.1 the preparation of rub(bing)test sample
Rub(bing)test adopts the some contact form, and last sample is alpha-sialon (Sialon) Ceramic Balls of Φ 8mm, the W18Cr4V steel that following sample is 19mm * 19mm.Wherein be carved with the ring groove of the dark 0.07mm of internal diameter 15mm external diameter 17mm at following sample friction surface.The solid lubricant powder at first grinds in agate mortar, then to going in the acetone, and disperses 15 minutes in the ultrasonic grinding machine.With dropper this acetone soln is dripped to following specimen surface again, treat that the complete back of acetone volatilization lubricant powder just is deposited on the surface of sample ring groove.
2.2 rub(bing)test method
Rub(bing)test adopts ball disc type high-temperature friction testing machine to carry out.Loading load is 980 Ns, 300 rev/mins of rotating speeds (linear velocity 0.24 meter per second), and temperature is between the room temperature to 500 ℃.Carried out in the test pure Ceramic Balls and steel when carrying out metal to-metal contact blank test and rub(bing)test when lubricated is arranged.
Embodiment 1
Tetrathio zinc molybdate (ZnMoS
4): get 0.5g (2.3mmol) Zn (Ac)
22H
2O is dissolved in the 20ml anhydrous methanol in 105 ℃ of oven dry down, and other gets 0.6g (2.3mmol) (NH
4)
2MoS
4Pour in the 250ml anhydrous methanol, under nitrogen protection, pulverize dissolving 30 minutes, after treating to dissolve fully, remove by filter impurity with the ultrasonic grinding machine, subsequently in nitrogen protection, and under agitation condition dropwise with Zn (Ac)
22H
2(NH during the methanol solution of O adds
4)
2MoS
4, wait to precipitate complete back and in 50 ℃ water-bath, be incubated, and keep and stirred 30 minutes.Centrifugation is removed impurity with the methanol wash precipitation, washs moisture and the methyl alcohol of removing wherein with anhydrous diethyl ether again.Under 70 ℃, dry to ether volatilization fully, a black solid, be tetrathio zinc molybdate (ZnMoS
4).First decomposition temperature is 236 ℃ in the air, and second decomposition temperature is 710 ℃.
Rub(bing)test result as shown in Figure 1
Fig. 1 is for there being tetrathio zinc molybdate (ZnMoS4) rub under the lubricated and unlubricated condition of powder Coefficient variation with temperature relation curve. Therefrom can find out in the blank assay Sialon Ceramic Balls with Steel its coefficient of friction when rubbing shows higher coefficient of friction (0.46), it in the time of 100 ℃ After descend to some extent, reach low value (0.18) during to 400 ℃ of left and right sides, begin again thereafter to rise. Corresponding, tetrathio zinc molybdate (ZnMoS is arranged4) under the lubricated condition of powder, whole Its coefficient of friction is all low than blank assay in the Range of measuring temp, and coefficient of friction changes Little. Wherein its coefficient of friction reaches low value (0.06) in the time of 100 ℃, rising then thereafter, Be 0.09 in the time of 400 ℃, then jump to maximum (0.18) during to 500 ℃.
Embodiment 2
Tetrathio barium molybdate (BaMoS
4): get 0.5g (2.04mmol) BaCl
22H
2O is dissolved in the 100ml anhydrous methanol in 105 ℃ of oven dry down, and other gets 0.5g (2.04mmol) (NH
4)
2MoS
4Pour in the 250ml anhydrous methanol, under nitrogen protection, pulverize dissolving 30 minutes, after treating to dissolve fully, remove by filter impurity with the ultrasonic grinding machine, subsequently in nitrogen protection, and dropwise will be dropwise with BaCl under agitation condition under agitation condition
22H
2The methanol solution of O adds (NH
4)
2MoS
4In, wait to precipitate complete back and in 50 ℃ water-bath, be incubated, and keep and stirred 30 minutes.Centrifugation is removed impurity with methanol wash precipitation, removes wherein moisture and methyl alcohol with the anhydrous diethyl ether washing again, under 70 ℃, dry to the ether volatilization fully, a black solid, be tetrathio barium molybdate (BaMoS
4).Its first decomposition temperature is 392 ℃ in the air, and second decomposition temperature is 686 ℃.
Friction test result as shown in Figure 2
Fig. 2 is for there being tetrathio barium molybdate (BaMoS4) rub under the lubricated and unlubricated condition of powder Coefficient variation with temperature relation curve. Can find out that therefrom tetrathio barium molybdate lubricious strip is arranged Under the part, it in the friction that whole temperature range coefficient of internal friction all is lower than under the DRY SLIDING is Number. Be 0.11 during room temperature, in the time of 100-400 ℃, its coefficient of friction changes steadily, is in 0.04-0.06 between. But its coefficient of friction rises to 0.14 in the time of 500 ℃.
Claims (3)
1. a tetrathiomolybdate is characterized in that compound is tetrathio zinc molybdate or tetrathio barium molybdate, and molecular formula is ZnMoS
4Or BaMoS
4
2. the preparation method of a tetrathiomolybdate is characterized in that getting respectively equimolar Zn (Ac)
22H
2O or BaCl
22H
2O and (NH
4)
2MoS
4Under nitrogen protection, be dissolved in the anhydrous methanol, treat that dissolving after-filtration fully removes impurity, under nitrogen, dropwise add Zn (Ac) again with the pulverizing of ultrasonic grinding machine
22H
2O or BaCl
22H
2The methanol solution of O, and keep stirring, wait to precipitate complete back and continue stirring and, isolate precipitation after the cooling in 50 ℃ of insulations 30 minutes, be product with oven dry after the methanol wash.
3. compound tetrathio zinc molybdate or tetrathio barium molybdate can be used as solid lubricant and use.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99121024A CN1095445C (en) | 1999-09-29 | 1999-09-29 | Tetrathiomolybdate, and its preparing process and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99121024A CN1095445C (en) | 1999-09-29 | 1999-09-29 | Tetrathiomolybdate, and its preparing process and application |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1266817A CN1266817A (en) | 2000-09-20 |
| CN1095445C true CN1095445C (en) | 2002-12-04 |
Family
ID=5281761
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN99121024A Expired - Fee Related CN1095445C (en) | 1999-09-29 | 1999-09-29 | Tetrathiomolybdate, and its preparing process and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1095445C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104556229B (en) * | 2014-12-31 | 2016-08-17 | 湖北大学 | A kind of environment-friendly preparation method thereof of four thio ammonium molybdate powder body |
| CN105296072A (en) * | 2015-12-02 | 2016-02-03 | 苏州捷德瑞精密机械有限公司 | Heatproof anti-rust lubricating oil and preparation method thereof |
| CN114042083B (en) * | 2021-12-06 | 2022-08-30 | 湖南师范大学 | Muscle-building and therapeutic applications of tetrathiomolybdate |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4283295A (en) * | 1979-06-28 | 1981-08-11 | Chevron Research Company | Process for preparing a sulfurized molybdenum-containing composition and lubricating oil containing said composition |
-
1999
- 1999-09-29 CN CN99121024A patent/CN1095445C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4283295A (en) * | 1979-06-28 | 1981-08-11 | Chevron Research Company | Process for preparing a sulfurized molybdenum-containing composition and lubricating oil containing said composition |
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| Publication number | Publication date |
|---|---|
| CN1266817A (en) | 2000-09-20 |
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