CN105834456A - Preparing method of nickel-coated molybdenum disulfide - Google Patents

Preparing method of nickel-coated molybdenum disulfide Download PDF

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Publication number
CN105834456A
CN105834456A CN201610309515.9A CN201610309515A CN105834456A CN 105834456 A CN105834456 A CN 105834456A CN 201610309515 A CN201610309515 A CN 201610309515A CN 105834456 A CN105834456 A CN 105834456A
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CN
China
Prior art keywords
preparation
liquid
molybdenum bisuphide
steam
nickel
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Pending
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CN201610309515.9A
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Chinese (zh)
Inventor
蔡兴明
程群
孙艳丽
钟明信
朱辉
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Jiangyou Hebao Nano Material Co Ltd
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Jiangyou Hebao Nano Material Co Ltd
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Priority to CN201610309515.9A priority Critical patent/CN105834456A/en
Publication of CN105834456A publication Critical patent/CN105834456A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
    • B22F9/305—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis of metal carbonyls
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/17—Metallic particles coated with metal

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Chemical Vapour Deposition (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses a preparing method of nickel-coated molybdenum disulfide. The preparing method comprises the following steps: (a), preparing a nickel raw material into Ni(CO)4 liquid; (b), vaporizing the Ni(CO)4 liquid into Ni(CO)4 steam; (c), leading the Ni(CO)4 steam into a coating furnace and carrying out vapor deposition coating on fluidized molybdenum disulfide powder by the Ni(CO)4 steam; and (d), obtaining carbonyl process nickel-coated molybdenum disulfide. According to the preparing method of the nickel-coated molybdenum disulfide, the carbonyl process nickel-coated molybdenum disulfide is prepared by a method for carrying out deposition coating on the fluidized molybdenum disulfide powder by the Ni(CO)4 steam. The utilizing rate of raw materials is high, the coating effect is great, the product is high in activity and stable in quality, and the method is easy to operate.

Description

The preparation method of nickel bag molybdenum bisuphide
Technical field
The present invention relates to the preparation method of composite, particularly relate to the preparation of nickel bag molybdenum bisuphide Method.
Background technology
Nickel bag molybdenum bisuphide is the most novel a kind of composite, can be applicable to corruption wear-resisting, anti- Field and the industries such as erosion, self-lubricating coat in use, oiliness bearing, dynamic sealing material and chemical industry, be Preferably antifriction material, is important kollag, and application prospect is good.Its preparation method master Electroless plating method to be had, Hydrothermal Pressure Hydrogen Reduction method, galvanoplastic etc..At present this product preparation method is ground Study carefully less, prepare nickel bag molybdenum bisuphide method in particular by carbonyl process and have no report, use carbonyl Base method prepares the method for nickel bag molybdenum bisuphide and product still belongs to blank, China can only rely on import or Do succedaneum with other material, hinder or have impact on the technological progress in the multiple field of China.
Summary of the invention
It is an object of the invention to overcome the above-mentioned deficiency in the presence of prior art, it is provided that nickel bag The preparation method of molybdenum bisuphide.
The present invention is achieved through the following technical solutions above-mentioned purpose:
The preparation method of nickel bag molybdenum bisuphide, comprises the following steps:
A the preparation of nickel raw material is become Ni (CO) by ()4Liquid；
B () is by Ni (CO)4Vaporizing liquid is Ni (CO)4Steam；
C () is by Ni (CO)4Steam is passed through in cladding stove and carries out gas with fluidization molybdenum bisuphide powder body Deposit cladding mutually；
D () obtains carbonyl process nickel bag molybdenum bisuphide.
As preferably, it is right that above-mentioned preparation method also includes after described step (a) completes Ni(CO)4Liquid carries out rectification, obtains high purity N i (CO)4Liquid.
As preferably, above-mentioned preparation method specifically includes following steps:
(1) nickel raw material is inserted autoclave, be passed through the CO gas of purity >=90%, Ni (CO) is prepared under conditions of air pressure 5～11.5MPa, temperature 120～150 DEG C4Liquid Body；
(2) to the Ni (CO) obtained4Liquid carries out rectification, obtains the weight/mass percentage composition of Fe Below 0.02%, the weight/mass percentage composition of the S high-purity below 0.01% Ni(CO)4Liquid；
(3) by Ni (CO)4Liquid imports heating vaporization in the carburator sealed, and obtains Ni(CO)4Steam；
(4) by Ni (CO)4Steam is passed through the N of purity >=99.9%2Gas, and by after vaporization Ni(CO)4Steam carrier band enters fluidization molybdenum bisuphide powder body cladding stove, in 260-350 DEG C carries out vapour deposition cladding, makes Ni (CO)4At molybdenum bisuphide powder body Surface is decomposed and deposits；
(5) the carbonyl process nickel bag molybdenum bisuphide after deposition cladding is obtained, and different by its granularity Carry out classification collection.
As preferably, the preferred 11MPa of above-mentioned steps (1) described air pressure, described temperature is excellent Select 130 DEG C.
As preferably, the temperature of above-mentioned steps (2) described rectification is preferably 44-60 DEG C. More preferably 48-56 DEG C.
As preferably, above-mentioned steps (3) vapourizing temperature is preferably 65-75 DEG C.Further It is preferably 67-72 DEG C.
As preferably, the granularity of above-mentioned steps (4) described molybdenum bisuphide powder body is preferably -46-+37ùm。
Compared with prior art, beneficial effects of the present invention: the system of nickel bag molybdenum bisuphide of the present invention Preparation Method is by by steam Ni (CO)4Method system with the deposition cladding of fluidization molybdenum bisuphide powder body Taking carbonyl process nickel bag molybdenum bisuphide, raw material availability is high, and total recovery reaches more than 98%, cladding Effective, cladding rate reaches more than 99%, and Product Activity is high, steady quality, and method easily operates.
Detailed description of the invention
Below in conjunction with test example and detailed description of the invention, the present invention is described in further detail. But this should not being interpreted as, the scope of the above-mentioned theme of the present invention is only limitted to below example, all bases The technology realized in present invention belongs to the scope of the present invention.
The preparation method of embodiment 1 nickel bag molybdenum bisuphide
The preparation method of nickel bag molybdenum bisuphide, inserts autoclave by nickel raw material, is passed through purity The CO gas of >=90%, prepares Ni (CO) under conditions of air pressure 11MPa, temperature 130 DEG C4Liquid Body；To the Ni (CO) obtained4Liquid carries out rectification, and rectification temperature is 50 ± 3 DEG C, obtains Fe Weight/mass percentage composition below 0.02%, the weight/mass percentage composition of S is below 0.01% High purity N i (CO)4Liquid；By Ni (CO)4Liquid imports heating vaporization in the carburator sealed, Vapourizing temperature is 69 DEG C, obtains Ni (CO)4Steam；By Ni (CO)4Steam passes through purity >=99.9% N2Gas, and by the Ni (CO) after vaporization4Steam carrier band enters fluidization molybdenum bisuphide powder body Cladding stove carries out vapour deposition cladding, and cladding furnace temperature is 297 DEG C, makes Ni (CO)4In curing Molybdenum powder surface is decomposed and deposits；Obtain the carbonyl process nickel bag curing after deposition cladding Molybdenum, and carry out classification collection by its particle diameter difference.Fluidization molybdenum bisuphide powder body described in this example Granularity is-46-+37 ù m, prepares according to standard GB/T23271-2009.
The example method raw material availability is high, and total recovery reaches more than 98%, clads effective, bag Multiple rate reaches more than 99%, and Product Activity is high, steady quality, and method easily operates.
The preparation method of embodiment 2 nickel bag molybdenum bisuphide
The preparation method of nickel bag molybdenum bisuphide, comprises the following steps:
(1) nickel raw material is inserted autoclave, be passed through the CO gas of purity >=90%, Air pressure11.5Ni (CO) is prepared under conditions of MPa, temperature 120 DEG C4Liquid；
(2) to the Ni (CO) obtained4Liquid carries out rectification, and rectification temperature is 44 DEG C, obtains The weight/mass percentage composition of Fe below 0.02%, the weight/mass percentage composition of S exists The high purity N i (CO) of less than 0.01%4Liquid；
(3) by Ni (CO)4Liquid imports heating vaporization in the carburator sealed, and vapourizing temperature is 75 DEG C, obtain Ni (CO)4Steam；
(4) by Ni (CO)4Steam is passed through the N of purity >=99.9%2Gas, and by after vaporization Ni(CO)4Steam carrier band enters fluidization molybdenum bisuphide powder body cladding stove, in 260 DEG C carry out vapour deposition cladding, make Ni (CO)4At molybdenum bisuphide powder surface Decomposing and deposit, the granularity of described fluidization molybdenum bisuphide powder body is -46-+37ùm；
(5) the carbonyl process nickel bag molybdenum bisuphide after deposition cladding is obtained, and different by its granularity Carry out classification collection.
The example method raw material availability is high, and total recovery reaches more than 98%, clads effective, bag Multiple rate reaches more than 99%, and Product Activity is high, steady quality, and method easily operates.
The preparation method of embodiment 3 nickel bag molybdenum bisuphide
The preparation method of nickel bag molybdenum bisuphide, comprises the following steps:
(1) nickel raw material is inserted autoclave, be passed through the CO gas of purity >=90%, Ni (CO) is prepared under conditions of air pressure 5MPa, temperature 150 DEG C4Liquid；
(2) to the Ni (CO) obtained4Liquid carries out rectification, rectification temperature 60 DEG C, obtains Fe Weight/mass percentage composition below 0.02%, the weight/mass percentage composition of S exists The high purity N i (CO) of less than 0.01%4Liquid；
(3) by Ni (CO)4Liquid imports heating vaporization, vapourizing temperature in the carburator sealed 65 DEG C, obtain Ni (CO)4Steam；
(4) by Ni (CO)4Steam is passed through the N of purity >=99.9%2Gas, and by after vaporization Ni(CO)4Steam carrier band enters fluidization molybdenum bisuphide powder body cladding stove, in 350 DEG C carry out vapour deposition cladding, make Ni (CO)4At molybdenum bisuphide powder surface Decomposing and deposit, the granularity of described fluidization molybdenum bisuphide powder body is -46-+37ùm；
(5) the carbonyl process nickel bag molybdenum bisuphide after deposition cladding is obtained, and different by its granularity Carry out classification collection.
The example method raw material availability is high, and total recovery reaches more than 98%, clads effective, bag Multiple rate reaches more than 99%, and Product Activity is high, steady quality, and method easily operates.
The preparation method of embodiment 4 nickel bag molybdenum bisuphide
The preparation method of nickel bag molybdenum bisuphide, comprises the following steps:
(1) nickel raw material is inserted autoclave, be passed through the CO gas of purity >=90%, Air pressure9.8Ni (CO) is prepared under conditions of MPa, temperature 135 DEG C4Liquid；
(2) to the Ni (CO) obtained4Liquid carries out rectification, rectification temperature 48 DEG C, obtains Fe Weight/mass percentage composition below 0.02%, the weight/mass percentage composition of S exists The high purity N i (CO) of less than 0.01%4Liquid；
(3) by Ni (CO)4Liquid imports heating vaporization, vapourizing temperature in the carburator sealed 70 DEG C, obtain Ni (CO)4Steam；
(4) by Ni (CO)4Steam is passed through the N of purity >=99.9%2Gas, and by after vaporization Ni(CO)4Steam carrier band enters fluidization molybdenum bisuphide powder body cladding stove, in 306 DEG C carry out vapour deposition cladding, make Ni (CO)4At molybdenum bisuphide powder surface Decomposing and deposit, the granularity of described fluidization molybdenum bisuphide powder body is -46-+37ùm；
(5) the carbonyl process nickel bag molybdenum bisuphide after deposition cladding is obtained, and different by its granularity Carry out classification collection.
The example method raw material availability is high, and total recovery reaches more than 98%, clads effective, bag Multiple rate reaches more than 99%, and Product Activity is high, steady quality, and method easily operates.

Claims (9)

1. the preparation method of nickel bag molybdenum bisuphide, it is characterised in that comprise the following steps:
A the preparation of nickel raw material is become Ni (CO) by ()4Liquid；
B () is by Ni (CO)4Vaporizing liquid is Ni (CO)4Steam；
C () is by Ni (CO)4Steam is passed through in cladding stove and carries out gas with fluidization molybdenum bisuphide powder body Deposit cladding mutually；
D () obtains carbonyl process nickel bag molybdenum bisuphide.
Preparation method the most according to claim 1, its feature is taken notice of, in described step A () also includes Ni (CO) after completing4Liquid carries out rectification, obtains high purity N i (CO)4Liquid Body.
Preparation method the most according to claim 2, it is characterised in that specifically include with Lower step:
(1) nickel raw material is inserted autoclave, be passed through the CO gas of purity >=90%, Air pressure5～under conditions of 11.5MPa, temperature 120～150 DEG C, prepare Ni (CO)4Liquid Body；
(2) to the Ni (CO) obtained4Liquid carries out rectification, obtains the weight/mass percentage composition of Fe Below 0.02%, the weight/mass percentage composition of the S high-purity below 0.01% Ni(CO)4Liquid；
(3) by Ni (CO)4Liquid imports heating vaporization in the carburator sealed, and obtains Ni(CO)4Steam；
(4) by Ni (CO)4Steam is passed through the N of purity >=99.9%2Gas, and by after vaporization Ni(CO)4Steam carrier band enters fluidization molybdenum bisuphide powder body cladding stove, in 260-350 DEG C carries out vapour deposition cladding, makes Ni (CO)4At molybdenum bisuphide powder body Surface is decomposed and deposits；
(5) the carbonyl process nickel bag molybdenum bisuphide after deposition cladding is obtained, and different by its granularity Carry out classification collection.
Preparation method the most according to claim 3, it is characterised in that described step (1) Described in air pressure be 11MPa, described temperature is 130 DEG C.
5. according to the preparation method described in claim 3 or 4, it is characterised in that described step Suddenly described in (2), the temperature of rectification is 44-60 DEG C.
Preparation method the most according to claim 5, it is characterised in that described step (2) Described in the temperature of rectification be 48-56 DEG C.
7. according to the preparation method described in claim 3 or 4, it is characterised in that described step Suddenly in (3), vapourizing temperature is 65-75 DEG C.
Preparation method the most according to claim 7, it is characterised in that described step (3) Middle vapourizing temperature is 67-72 DEG C.
9. according to the preparation method described in claim 3 or 4, it is characterised in that described step Suddenly the granularity of molybdenum bisuphide powder body described in (4) is-46-+37 ù m.
CN201610309515.9A 2016-05-11 2016-05-11 Preparing method of nickel-coated molybdenum disulfide Pending CN105834456A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107216685A (en) * 2017-06-21 2017-09-29 嵩县开拓者钼业有限公司 A kind of preparation method of the dustless molybdenum disulfide of lubricating additive
CN109023132A (en) * 2018-08-16 2018-12-18 镇江朝阳机电科技有限公司 A kind of elevator safety gear voussoir and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH02111804A (en) * 1988-10-20 1990-04-24 Mitsubishi Petrochem Co Ltd Manufacture of magnetic metal powder
CN1775424A (en) * 2005-12-15 2006-05-24 钢铁研究总院 Method for preparing solid self-lubricating material
CN102717067A (en) * 2012-06-05 2012-10-10 金川集团股份有限公司 Method for preparing nickel-coated powder
CN103394688A (en) * 2013-07-29 2013-11-20 中国钢研科技集团有限公司 Heatproof anti-wear self-lubrication material and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH02111804A (en) * 1988-10-20 1990-04-24 Mitsubishi Petrochem Co Ltd Manufacture of magnetic metal powder
CN1775424A (en) * 2005-12-15 2006-05-24 钢铁研究总院 Method for preparing solid self-lubricating material
CN102717067A (en) * 2012-06-05 2012-10-10 金川集团股份有限公司 Method for preparing nickel-coated powder
CN103394688A (en) * 2013-07-29 2013-11-20 中国钢研科技集团有限公司 Heatproof anti-wear self-lubrication material and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107216685A (en) * 2017-06-21 2017-09-29 嵩县开拓者钼业有限公司 A kind of preparation method of the dustless molybdenum disulfide of lubricating additive
CN109023132A (en) * 2018-08-16 2018-12-18 镇江朝阳机电科技有限公司 A kind of elevator safety gear voussoir and preparation method thereof

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