CN1124718A - Process for preparing superfine scale crystal tungsten disulfide - Google Patents
Process for preparing superfine scale crystal tungsten disulfide Download PDFInfo
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- CN1124718A CN1124718A CN 94119657 CN94119657A CN1124718A CN 1124718 A CN1124718 A CN 1124718A CN 94119657 CN94119657 CN 94119657 CN 94119657 A CN94119657 A CN 94119657A CN 1124718 A CN1124718 A CN 1124718A
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Abstract
The process for preparing ultrafine flaky crystal of WS2 as lubricant includes such steps as under condition of isolating air, heating and decomposing ammonium tetrathiammonium tungstate from room temp. to 700-1200 deg.C with temp. gradient of 100-200 deg.C/hr, keeping temp. at 700-1200 deg.C for 24-48 hr, cooling to room temp. with temp. gradient of 30-110 deg.C/hr, then exiting and breaking, and features no environmental pollution, stable quality, and safe and reliable operation.
Description
The present invention relates to a kind of preparation method of tungsten compound, a kind of more precisely preparation method who is used for the superfine scale crystal tungsten disulfide of lubricant.
The production method of tungsten disulfide has tetrathio ammonium tungstate oxidizing roasting decomposition method, acidifying thermal decomposition method, but the tungsten disulfide purity that above-mentioned two kinds of methods are produced is low, crystalline structure is not hexagonal system, does not satisfy the demand that on city's field boundary high purity, crystalline structure is the ultra-fine flaky tungsten disulfide of hexagonal system.
American documentation literature US3,725,276 have introduced the method for the crystallization tungsten disulfide that a kind of preparation is used to lubricate, its method is that the metal tungsten powder with the sulphur of 2-8mol and 1mol mixes mutually, form the mixture of sulphur and metal tungsten powder, this mixture is reacted under the temperature of the fusing point to 250 of sulphur ℃, again reactant is carried out crystallization under 550-650 ℃ temperature in nonoxidizing atmosphere, superfluous sulphur is removed in final evaporation
The Japanese documentation spy opens the manufacture method that clear 47-462293 has also introduced the ultra-fine lubricant tungsten disulfide of a kind of solid, its method is the mixture with metal tungsten powder and sulphur, temperature heating below the boiling point of sulphur, sulphur and metal tungsten powder reaction in liquid phase sulphur, then the tungsten disulfide that generates is injected into and gives heat to 550-650 ℃ container, thermopositive reaction takes place in this moment, makes the tungsten disulfide recrystallize of generation, simultaneously the sulphur evaporation is removed.
Because above-mentioned two pieces of patent documentations are technical scheme patent application documents two different national applications patents, the preparation method that the preparation of being narrated is used for the crystalloid tungsten disulfide of lubricant is identical, the height of used raw material tungsten, the purity requirement of sulphur, the purity of raw material tungsten is up to 99.98%, the purity of raw material sulphur is more than 99.95%, the material purity high price is expensive, technology more complicated, the product cost height of producing.
The objective of the invention is to work out a kind of new compound by tungsten is raw material, makes the technology of the tungsten disulfide of the ultra-fine squamous hexagonal system that is used to lubricate, and makes technology simple, easy handling, low cost product.
The preparation method of a kind of superfine scale crystal tungsten disulfide of the present invention, with the tetrathio ammonium tungstate is raw material, under the condition of secluding air, thermal degradation tetrathio ammonium tungstate, thermograde with 100-200 ℃/hour during heating is warming up to 700 ℃-1200 ℃ from room temperature, and under 700-1200 ℃ temperature, kept constant temperature 24-48 hour, reduce to room temperature with 30-110 ℃/hour thermograde again, and make superfine scale crystal tungsten disulfide of the present invention.
Used raw material tetrathio ammonium tungstate can be commercially available, the also method that can all know with the those of ordinary skill under this area, in the solution of ammonium tungstate, feed hydrogen sulfide and generate the tetrathio ammonium tungstate, again with tetrathio ammonium tungstate drying and crushing, the granularity of used tetrathio ammonium tungstate is less than 460m μ (less than 40 orders), content of impurities is less than 0.08% (weight percentage, down together), moisture less than 12% for well, granularity with the tetrathio ammonium tungstate is 50 μ m-300 μ m again, content of impurities is less than 0.05%, moisture content less than 10% for better, the granularity of its raw material is thin more good more, the total content of impurity is low more good more, moisture content is less than 8% the best, during thermal degradation tetrathio ammonium tungstate, thermograde with 100-200 ℃/hour, be warming up to 700 ℃-1200 ℃ from room temperature, again to be warming up to 900-1200 ℃, keep 30-48 hour homothermic time for well at 900-1200 ℃, reduce to room temperature with 30-110 ℃/hour thermograde again, it serves as better reducing to room temperature with 50-110 ℃/hour thermograde again, to the crystalline structure of producing is that the ultra-fine squamous tungsten disulfide product of hexagonal is pulverized, making its granularity is 2-20 μ m, its purity is 99.50-99.99%, and product proves hexagonal through X light diffracting analysis, sees Fig. 1.
The superfine scale crystal tungsten disulfide made from method of the present invention has higher thermotolerance, barotolerance, and oilness, fully applicable to high rotating speed, high pressure, the needs of the lubricant of high vacuum and high temperature or low temperature sudden change part.
Used equipment is electric calcination stove (commercially available) in the technology of the present invention, the airtight gas that is produced when wanting reliably only to discharge roasting, and air is advanced in inaccurate leakage.
The preparation method's of superfine scale crystal tungsten disulfide of the present invention advantage is:
1. method processing unit of the present invention is simple, and device just wants electric calcination stove, the less investment of founding the factory, processing condition can adopt the control of self-acting control device, and operational safety is reliable, the tungsten disulfide that can to produce stay-in-grade high pure and ultra-fine crystalline structure again be hexagonal system.
2. because the equipment that adopted is airtight, the processing of the obnoxious flavour that produces when being convenient to roasting, good operational environment, free from environmental pollution.
Fig. 1 product tungsten disulfide X-ray diffraction spectrogram
X-coordinate is 2 θ angles, and ordinate zou is counting (cps)
With following embodiment the preparation method of superfine scale crystal tungsten disulfide of the present invention is further described; to help understanding to the present invention and advantage thereof; and not as the qualification to protection scope of the present invention, protection scope of the present invention is decided by claim.
Embodiment 1
With water content 5%, content of impurities is that 0.03% tetrathio ammonium tungstate is a raw material, the granularity of tetrathio ammonium tungstate is less than 460m μ (crossing 40 orders), raw material tetrathio ammonium tungstate is placed electric calcination stove, secluding air carries out airtight roast, thermograde with 114.5 ℃/hour, be warming up to 1120 ℃ from room temperature, keep constant temperature after 27 hours at 1120 ℃, reduce to room temperature with 47.3 ℃/hour thermograde again, discharging is pulverized, and the tungsten disulfide purity of producing is 99.63%, granularity is 2-20 μ m, for being the hexagonal system tungsten disulfide.
Embodiment 2
Its working method and condition are substantially with embodiment 1, only different is that moisture content is 5% in the tetrathio ammonium tungstate, and content of impurities is 0.003%, and its granularity is less than 460m μ (crossing 40 orders), thermograde with 120 ℃/hour, be warming up to 1050 ℃ from room temperature, kept constant temperature 27 hours, reduce to room temperature with 35 ℃/hour thermograde again at 1050 ℃, discharging is pulverized, the tungsten disulfide purity of producing is 99.93%, and granularity is 2-20 μ m, for being the tungsten disulfide of hexagonal system.
Embodiment 3
Its working method and condition are substantially with embodiment 1, only different is that moisture content is 7.2% in the tetrathio ammonium tungstate, content of impurities is 0.001%, and its granularity is less than 460m μ (crossing 40 orders), is warming up to 960 ℃ with 185 ℃/hour thermogrades, keep constant temperature after 32 hours at 960 ℃, reduce to room temperature with 65 ℃/hour thermograde again, discharging is pulverized, and product purity is 99.97%, granularity is 2-20 μ m, for being the tungsten disulfide of hexagonal system.
Embodiment 4
Its working method and condition are substantially with embodiment 1, only different is that moisture content is 7.2% in the tetrathio ammonium tungstate, content of impurities is 0.041%, and its granularity is less than 460m μ (crossing 40 orders), is warming up to 1180 ℃ with 168.6 ℃/hour thermogrades, keep constant temperature after 32 hours at 1180 ℃, reduce to room temperature with 42.1 ℃/hour thermograde again, discharging is pulverized, and product purity is 99.58%, granularity is 2-20 μ m, for being the tungsten disulfide of hexagonal system.
Embodiment 5
Its working method and condition are substantially with embodiment 1, only different is that moisture content is 8% in the tetrathio ammonium tungstate, content of impurities is 0.027%, its granularity is less than 460m μ (crossing 40 orders), be warming up to 1050 ℃ with 116.7 ℃/hour thermogrades, keep constant temperature after 43 hours at 1050 ℃, reduce to room temperature with 42 ℃/hour thermograde again, discharging is pulverized; Product purity is 99.96%, and granularity is 2-20 μ m, for being the tungsten disulfide of hexagonal system.
Embodiment 6
Its working method and condition are substantially with embodiment 1, only different is that moisture content is 8% in the tetrathio ammonium tungstate, content of impurities is 0.017%, and its granularity is less than 460m μ (crossing 40 orders), is warming up to 840 ℃ with 152 ℃/hour thermogrades, keep constant temperature after 43 hours at 840 ℃, reduce to room temperature with 80 ℃/hour thermograde again, discharging is pulverized, and product purity is 99.98%, granularity is 2-20 μ m, for being the tungsten disulfide of hexagonal system.
Claims (8)
1. the preparation method of a superfine scale crystal tungsten disulfide, it is characterized in that, with the tetrathio ammonium tungstate is raw material, under the condition of secluding air, thermal degradation tetrathio ammonium tungstate, thermograde with 100-200 ℃/hour during heating rises to 700-1200 from room temperature, and keeps constant temperature 24-48 hour under 700-1200 ℃ temperature, reduces to room temperature with 30-110 ℃/hour thermograde again.
2. according to the preparation method of a kind of tungsten disulfide of claim 1, it is characterized in that the granularity of tetrathio ammonium tungstate is less than 460 μ m.
3. according to the preparation method of a kind of tungsten disulfide of claim 1, it is characterized in that tetrathio ammonium tungstate content of impurities is less than 0.08% (weight percentage, down with), moisture content is less than 12%.
4, according to the preparation method of a kind of tungsten disulfide of claim 2, it is characterized in that the granularity of tetrathio ammonium tungstate is 50-300 μ m.
5. according to the preparation method of a kind of tungsten disulfide of claim 3, it is characterized in that tetrathio ammonium tungstate content of impurities is less than 0.05%, moisture content is less than 10%,
6. according to the preparation method of a kind of tungsten disulfide of claim 1, it is characterized in that, rise to 900-1200 ℃ from room temperature, under 900-1200 ℃ temperature, kept constant temperature 30-48 hour with 100-200 ℃/hour thermograde.
7. according to the preparation method of a kind of tungsten disulfide of claim 1, it is characterized in that, reduce to room temperature with 50-110 ℃/hour thermograde.
8, the preparation method according to a kind of tungsten disulfide of claim 1 is characterized in that, the tungsten disulfide product is pulverized, and making its granularity is 2-20 μ m.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94119657 CN1124718A (en) | 1994-12-16 | 1994-12-16 | Process for preparing superfine scale crystal tungsten disulfide |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 94119657 CN1124718A (en) | 1994-12-16 | 1994-12-16 | Process for preparing superfine scale crystal tungsten disulfide |
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| CN1124718A true CN1124718A (en) | 1996-06-19 |
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| CN 94119657 Pending CN1124718A (en) | 1994-12-16 | 1994-12-16 | Process for preparing superfine scale crystal tungsten disulfide |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103420423A (en) * | 2013-08-09 | 2013-12-04 | 深圳市威勒达科技开发有限公司 | Preparation method for tungsten disulfide |
| CN104695021A (en) * | 2015-03-05 | 2015-06-10 | 湖南大学 | Lamellar helical WS2 two-dimensional nano material and preparation method thereof |
| CN113023780A (en) * | 2021-03-17 | 2021-06-25 | 李伟强 | Nanoscale tungsten disulfide material, preparation method and preparation device thereof |
-
1994
- 1994-12-16 CN CN 94119657 patent/CN1124718A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103420423A (en) * | 2013-08-09 | 2013-12-04 | 深圳市威勒达科技开发有限公司 | Preparation method for tungsten disulfide |
| CN103420423B (en) * | 2013-08-09 | 2015-05-13 | 深圳市威勒达科技开发有限公司 | Preparation method for tungsten disulfide |
| CN104695021A (en) * | 2015-03-05 | 2015-06-10 | 湖南大学 | Lamellar helical WS2 two-dimensional nano material and preparation method thereof |
| CN104695021B (en) * | 2015-03-05 | 2017-03-01 | 湖南大学 | A kind of stratiform spiral WS2Two-dimension nano materials and preparation method thereof |
| CN113023780A (en) * | 2021-03-17 | 2021-06-25 | 李伟强 | Nanoscale tungsten disulfide material, preparation method and preparation device thereof |
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