CN107418251A - A kind of anti-oxidation treatment method of ultra-fine molybdenum disulfide - Google Patents
A kind of anti-oxidation treatment method of ultra-fine molybdenum disulfide Download PDFInfo
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- CN107418251A CN107418251A CN201710765990.1A CN201710765990A CN107418251A CN 107418251 A CN107418251 A CN 107418251A CN 201710765990 A CN201710765990 A CN 201710765990A CN 107418251 A CN107418251 A CN 107418251A
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- molybdenum disulfide
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- treatment method
- oxidation treatment
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/0003—Compounds of molybdenum
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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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
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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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
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/90—Other properties not specified above
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Lubricants (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of anti-oxidation treatment method of ultra-fine molybdenum disulfide, specifically implement according to following steps：Step 1, prepare a certain amount of absolute ethyl alcohol, a certain amount of T5060 is instilled in absolute ethyl alcohol, stirring, form transparent lysate；Or prepare a certain amount of absolute methanol, a certain amount of T5057 is instilled in absolute methanol, stirring, forms transparent lysate；Step 2, lysate step 1 obtained is added in molybdenum disulfide, is stirred, and is well mixed, is obtained mixed liquor；Step 3, the obtained mixed liquor filtering in step 2, separation of solid and liquid, solid are put into vacuum drying chamber drying, obtain the molybdenum disulfide handled through anti-oxidant treatment.It is an object of the invention to provide a kind of anti-oxidation treatment method of ultra-fine molybdenum disulfide, solve the problems, such as that oxygen content present in prior art is exceeded.
Description
Technical field
The invention belongs to metallurgical technology technical field, is related to a kind of anti-oxidation treatment method of ultra-fine molybdenum disulfide.
Background technology
Molybdenum disulfide in compound grease, is dispersed in grease as lubricant additive with heterogeneity state.Its granularity
Influence to lubricant effect and application is very big, and as molybdenum disulfide particle diameter diminishes, specific surface area increase, it is attached on material
The property also significantly improves with level of coverage；Meanwhile granule number increases severely, the dispersiveness also obvious increase in grease, service life
Also it is longer, it also more can protect not frayed by lubriation material, the confirmations of various conditions, the small molybdenum disulfide of particle diameter has excellent resistance to
Mill property.
Usually used molybdenum disulfide particle diameter is at 20~30 μm, to requiring strict lubrication then 1~2 μm of even 1 μ on request
Below m powder, such as, imported car h type engine h should be less than 1~3 μm with addition particle diameter in molybdenum disulphide grease.Lubricating oil adds
Easily deposited when granularity is big when adding molybdenum disulfide and easily block oil circuit and oil filter, therefore require that addition is less than 1 μm even less than 1 μm
Molybdenum disulfide.
Though fine granularity has high lubricant effect, as granularity reduces, specific surface area increases, increase with oxygen contact area
Greatly, oxidation rate improves rapidly in an atmosphere, and friction industry confirms extensively, when molybdenum disulfide is oxidized to molybdenum oxide, lubrication
Failure, the general oxygen content for requiring (1~2 μm of granularity) molybdenum disulfide is (with MoO3Meter) it is no more than 0.3%, acid number is no more than 3%,
Oil content is no more than 0.5%.Being found in actual production, after molybdenum disulfide places a period of time, oxygen content is exceeded, or even sometimes
For product upon producing, oxygen content is exceeded.
The content of the invention
It is an object of the invention to provide a kind of anti-oxidation treatment method of ultra-fine molybdenum disulfide, solve and deposit in the prior art
Oxygen content it is exceeded the problem of.
The technical solution adopted in the present invention is a kind of anti-oxidation treatment method of ultra-fine molybdenum disulfide, specifically according to
Lower step is implemented：
Step 1, prepare a certain amount of absolute ethyl alcohol, a certain amount of T5060 is instilled in absolute ethyl alcohol, stirring, formed saturating
Bright lysate；Or prepare a certain amount of absolute methanol, a certain amount of T5057 is instilled in absolute methanol, stirring, formed transparent
Lysate；
Step 2, lysate step 1 obtained is added in molybdenum disulfide, is stirred, and is well mixed, is obtained mixed liquor；
Step 3, the obtained mixed liquor filtering in step 2, separation of solid and liquid, solid are put into vacuum drying chamber drying, obtained
To the molybdenum disulfide handled through anti-oxidant treatment.
The features of the present invention also resides in,
The mass ratio of T5060 and absolute ethyl alcohol is 1 in step 1：250~1200.
The mass ratio of T5057 and absolute methanol is 1 in step 1：250~1200.
When step 1 is prepares a certain amount of absolute ethyl alcohol, a certain amount of T5060 is instilled in absolute ethyl alcohol, stirred, is formed
During transparent lysate：
Molybdenum disulfide Fisher particle size Fsss=0.3~0.5 μm in step 2；
The mass ratio of molybdenum disulfide and lysate in step 2 is 1：0.7~1；
The operating temperature of vacuum drying chamber in step 3 is 40~50 DEG C, and drying time is 5~8h.
When step 1 is prepares a certain amount of absolute methanol, a certain amount of T5057 is instilled in absolute methanol, stirred, is formed
During transparent lysate：
Molybdenum disulfide granularity D in step 250=0.6~2 μm；
The mass ratio of lysate and molybdenum disulfide in step 2 is 1：1.67~2.5.
The operating temperature of vacuum drying chamber in step 3 is 40~60 DEG C, and drying time is 2~4h.
The invention has the advantages that the method for the present invention can form thin oil film on molybdenum disulfide particles surface, effectively
Prevent from being oxidized in molybdenum disulfide air, while again minimize oil content, and ensure other indexs without departing from requiring, it is ensured that under
Swim the production of lubricant.
Embodiment
With reference to embodiment, the present invention is described in detail.
A kind of anti-oxidation treatment method of ultra-fine molybdenum disulfide, specifically implements according to following steps：
Step 1, prepare a certain amount of absolute ethyl alcohol, a certain amount of T5060 is instilled in absolute ethyl alcohol, stirring, formed saturating
The mass ratio of bright lysate, wherein T5060 and absolute ethyl alcohol is 1：250~1200；
Step 2, lysate step 1 obtained is added in molybdenum disulfide, is stirred, and is well mixed, is obtained mixed liquor, its
The mass ratio of middle molybdenum disulfide Fisher particle size Fsss=0.3~0.5 μm, molybdenum disulfide and lysate is 1：0.7~1；
Step 3, the obtained mixed liquor filtering in step 2, separation of solid and liquid, solid are put into vacuum drying chamber drying, with
Operating temperature is 40~50 DEG C, dries 5~8h, obtains the molybdenum disulfide handled through anti-oxidant treatment.
A kind of anti-oxidation treatment method of ultra-fine molybdenum disulfide, specifically implements according to following steps：
Step 1, prepare a certain amount of absolute methanol, a certain amount of T5057 is instilled in absolute methanol, stirring, formed saturating
The mass ratio of bright lysate, wherein T5057 and absolute methanol is 1：250~1200；
Step 2, lysate step 1 obtained is added in molybdenum disulfide, is stirred, and is well mixed, is obtained mixed liquor, its
In, molybdenum disulfide granularity D50=0.6~2 μm, the mass ratio of lysate and molybdenum disulfide is 1：1.67~2.5；
Step 3, the obtained mixed liquor filtering in step 2, separation of solid and liquid, solid are put into vacuum drying chamber drying, with
Operating temperature is 40~60 DEG C, dries 2~4h, obtains the molybdenum disulfide handled through anti-oxidant treatment.
The T5060 of the present invention is liquid mixing dialkyl diphenylamine, and a kind of efficient high-temperature antioxidant is thick light yellow
Oil, insoluble in ether, ketone.Very small amount T5060 is directly added into molybdenum disulfide, it is uniformly dispersed and is no more than oil content
0.5% is difficult, and the present invention is that T5060 is dissolved in absolute ethyl alcohol, the big lysate of forming amount, then adds ultra-fine two
In molybdenum sulfide, drying, layer protecting film is formed in particle surface after volatilization.
The T5057 of the present invention is liquid mixing dialkyl diphenylamine, and a kind of efficient high-temperature antioxidant is thick light yellow
Oil, insoluble in ether, ketone.Very small amount T5057 is directly added into molybdenum disulfide, it is uniformly dispersed and is no more than oil content
0.5% is difficult, and the application patent is that T5057 is dissolved in absolute methanol, the big lysate of forming amount, then adds two
In molybdenum sulfide, drying, layer protecting film is formed in particle surface after volatilization.
Embodiment 1
A kind of anti-oxidation treatment method of ultra-fine molybdenum disulfide, specifically implements according to following steps：
Step 1, prepare absolute ethyl alcohol, T5060 is instilled wherein, the mass ratio of T5060 and absolute ethyl alcohol is 1：250, stir
Mix, form transparent lysate；
Step 2, lysate step 1 obtained is added in molybdenum disulfide, is stirred, and is well mixed, is obtained mixed liquor, wherein
The mass ratio of Fsss=0.3 μm of the Fisher particle size of molybdenum disulfide, molybdenum disulfide and lysate is 1：1；
Step 3, mixed liquor step 2 obtained filters, separation of solid and liquid, and solid is put into vacuum drying chamber drying, temperature 40
DEG C drying 8h.
Table 1 is that same raw material is as follows without anti-oxidant treatment (blank) and the result after the processing of example 1：The oxygen of example 1 contains
The indices such as amount are without departing from production requirement.
Table 1
Embodiment 2
A kind of anti-oxidation treatment method of ultra-fine molybdenum disulfide, specifically implements according to following steps：
Step 1, prepare absolute ethyl alcohol, T5060 is instilled wherein, wherein, the mass ratio of T5060 and absolute ethyl alcohol is 1：
400, stirring, form transparent lysate；
Step 2, lysate is added in molybdenum disulfide, stirred, be well mixed, obtain mixed liquor, wherein, molybdenum disulfide
The mass ratio of Fsss=0.4 μm of Fisher particle size, molybdenum disulfide and lysate is 1：0.85；
Step 3, mixed liquor step 2 obtained filters, separation of solid and liquid, and solid is put into vacuum drying chamber drying, with temperature
45 DEG C of dry 6.5h.
Table 2 is that same raw material is as follows with the result that is handled through example 2 without anti-oxidant treatment (blank), and the oxygen of example 2 contains
The indices such as amount are without departing from production requirement.
Table 2
Embodiment 3
A kind of anti-oxidation treatment method of ultra-fine molybdenum disulfide, specifically implements according to following steps：
Step 1, prepare absolute ethyl alcohol, T5060 is instilled wherein, stirring, forms transparent lysate, wherein, T5060 and nothing
The mass ratio of water-ethanol is 1：1200；
Step 2, lysate is added in molybdenum disulfide, stirred, be well mixed, obtain mixed liquor, wherein, molybdenum disulfide
The mass ratio of Fsss=0.5 μm of Fisher particle size, molybdenum disulfide and lysate is 1：0.7；
Step 3, mixed liquor step 2 obtained filters, separation of solid and liquid, and solid is put into vacuum drying chamber drying, with temperature
50 DEG C of dry 5h.
Table 3 is that same raw material is as follows with the result that is handled through example 3 without anti-oxidant treatment (blank), and the oxygen of example 3 contains
The indices such as amount are without departing from production requirement.
Table 3
Embodiment 4
A kind of anti-oxidation treatment method of ultra-fine molybdenum disulfide, specifically implements according to following steps：
Step 1, prepare absolute methanol, T5057 is instilled wherein, stirring, forms transparent lysate, wherein, T5057 and nothing
The mass ratio of water methanol is 1：250；
Step 2, lysate is added in molybdenum disulfide, stirred, be well mixed, obtain mixed liquor, wherein, molybdenum disulfide grain
Spend D50=0.66 μm, the mass ratio of lysate and molybdenum disulfide is 1：1.67；
Step 3, mixed liquor step 2 obtained filters, separation of solid and liquid, and solid is put into vacuum drying chamber drying, with temperature
40 DEG C of drying 2h.
Table 4 is that same raw material is as follows with the result that is handled through example 4 without anti-oxidant treatment (blank), and the oxygen of example 4 contains
The indices such as amount are without departing from production requirement.
Table 4
Embodiment 5
A kind of anti-oxidation treatment method of ultra-fine molybdenum disulfide, specifically implements according to following steps：
Step 1, prepare absolute methanol, T5057 is instilled wherein, stirring, forms transparent lysate, wherein, T5057 and nothing
The mass ratio of water methanol is 1：400；
Step 2, lysate is added in molybdenum disulfide, stirred, be well mixed, obtain mixed liquor, wherein, molybdenum disulfide grain
Spend D50=0.77 μm, the mass ratio of lysate and molybdenum disulfide is 1：2；
Step 3, mixed liquor step 2 obtained filters, separation of solid and liquid, and solid is put into vacuum drying chamber drying, with temperature
50 DEG C of dry 3h.
Table 5 is that same raw material is as follows with the result that is handled through example 5 without anti-oxidant treatment (blank), and the oxygen of example 5 contains
The indices such as amount are without departing from production requirement.
Table 5
Embodiment 6
A kind of anti-oxidation treatment method of ultra-fine molybdenum disulfide, specifically implements according to following steps：
Step 1, prepare absolute methanol, T5057 is instilled wherein, stirring, forms transparent lysate, wherein, T5057 and nothing
The mass ratio of water methanol is 1：1200；
Step 2, lysate is added in molybdenum disulfide, stirred, be well mixed, obtain mixed liquor, wherein, molybdenum disulfide grain
Spend D50=1.17 μm, the mass ratio of lysate and molybdenum disulfide is 1：2.5；
Step 3, mixed liquor step 2 obtained filters, separation of solid and liquid, and solid is put into vacuum drying chamber drying, with temperature
60 DEG C of dry 4h.
Table 6 is that same raw material is as follows with the result that is handled through example 6 without anti-oxidant treatment (blank), and the oxygen of example 6 contains
The indices such as amount are without departing from production requirement.
Table 6
Claims (9)
1. a kind of anti-oxidation treatment method of ultra-fine molybdenum disulfide, it is characterised in that specifically implement according to following steps：
Step 1, prepare a certain amount of absolute ethyl alcohol, a certain amount of T5060 is instilled in absolute ethyl alcohol, stirring, formed transparent molten
Solve liquid；Or prepare a certain amount of absolute methanol, a certain amount of T5057 is instilled in absolute methanol, stirring, forms transparent dissolving
Liquid；
Step 2, lysate step 1 obtained is added in molybdenum disulfide, is stirred, and is well mixed, is obtained mixed liquor；
Step 3, the mixed liquor filtering of obtaining in step 2, separation of solid and liquid, solid are put into vacuum drying chamber drying, obtain through
The molybdenum disulfide of anti-oxidant treatment processing.
2. the anti-oxidation treatment method of a kind of ultra-fine molybdenum disulfide according to claim 1, it is characterised in that in step 1
The mass ratio of the T5060 and absolute ethyl alcohol are 1：250~1200.
3. the anti-oxidation treatment method of a kind of ultra-fine molybdenum disulfide according to claim 1, it is characterised in that in step 1
The mass ratio of the T5057 and absolute methanol are 1：250~1200.
4. the anti-oxidation treatment method of a kind of ultra-fine molybdenum disulfide according to claim 1, it is characterised in that when step 1
To prepare a certain amount of absolute ethyl alcohol, a certain amount of T5060 is instilled in absolute ethyl alcohol, stirring, when forming transparent lysate, step
Molybdenum disulfide Fisher particle size Fsss=0.3~0.5 μm described in rapid 2.
5. the anti-oxidation treatment method of a kind of ultra-fine molybdenum disulfide according to claim 1, it is characterised in that when step 1
To prepare a certain amount of absolute methanol, a certain amount of T5057 is instilled in absolute methanol, stirring, when forming transparent lysate, step
Molybdenum disulfide granularity D described in rapid 250=0.6~2 μm.
6. the anti-oxidation treatment method of a kind of ultra-fine molybdenum disulfide according to claim 4, it is characterised in that in step 2
Described molybdenum disulfide and the mass ratio of lysate are 1：0.7~1.
7. the anti-oxidation treatment method of a kind of ultra-fine molybdenum disulfide according to claim 5, it is characterised in that in step 2
Described lysate and the mass ratio of molybdenum disulfide are 1：1.67~2.5.
8. the anti-oxidation treatment method of a kind of ultra-fine molybdenum disulfide according to claim 6, it is characterised in that in step 3
The operating temperature of described vacuum drying chamber is 40~50 DEG C, and drying time is 5~8h.
9. the anti-oxidation treatment method of a kind of ultra-fine molybdenum disulfide according to claim 7, it is characterised in that in step 3
The operating temperature of described vacuum drying chamber is 40~60 DEG C, and drying time is 2~4h.
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| CN201710765990.1A CN107418251B (en) | 2017-08-30 | 2017-08-30 | Oxidation-resistant treatment method for superfine molybdenum disulfide |
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| CN201710765990.1A CN107418251B (en) | 2017-08-30 | 2017-08-30 | Oxidation-resistant treatment method for superfine molybdenum disulfide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111925668A (en) * | 2020-07-14 | 2020-11-13 | 申雨润滑科技有限公司 | Intercalation inlaid coated oil-soluble molybdenum-based lubricating oil additive and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111925668A (en) * | 2020-07-14 | 2020-11-13 | 申雨润滑科技有限公司 | Intercalation inlaid coated oil-soluble molybdenum-based lubricating oil additive and preparation method thereof |
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| CN107418251B (en) | 2020-08-25 |
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