CN1240765A - Synthesis method of high-purity nickel disulfide powder - Google Patents
Synthesis method of high-purity nickel disulfide powder Download PDFInfo
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- CN1240765A CN1240765A CN 99109781 CN99109781A CN1240765A CN 1240765 A CN1240765 A CN 1240765A CN 99109781 CN99109781 CN 99109781 CN 99109781 A CN99109781 A CN 99109781A CN 1240765 A CN1240765 A CN 1240765A
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- 239000000843 powder Substances 0.000 title claims abstract description 26
- NKHCNALJONDGSY-UHFFFAOYSA-N nickel disulfide Chemical compound [Ni+2].[S-][S-] NKHCNALJONDGSY-UHFFFAOYSA-N 0.000 title abstract 3
- 238000001308 synthesis method Methods 0.000 title 1
- 238000000034 method Methods 0.000 claims abstract description 13
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 13
- 239000005864 Sulphur Substances 0.000 claims description 10
- 239000012043 crude product Substances 0.000 claims description 4
- 238000010189 synthetic method Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000047 product Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 229910000339 iron disulfide Inorganic materials 0.000 abstract description 2
- 238000007789 sealing Methods 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- XUKVMZJGMBEQDE-UHFFFAOYSA-N [Co](=S)=S Chemical compound [Co](=S)=S XUKVMZJGMBEQDE-UHFFFAOYSA-N 0.000 abstract 1
- NFMAZVUSKIJEIH-UHFFFAOYSA-N bis(sulfanylidene)iron Chemical compound S=[Fe]=S NFMAZVUSKIJEIH-UHFFFAOYSA-N 0.000 abstract 1
- 239000010419 fine particle Substances 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 239000000463 material Substances 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
- Glass Compositions (AREA)
Abstract
The invention discloses a method for synthesizing high-purity nickel disulfide powder, which comprises the steps of taking high-purity elemental nickel powder and sulfur powder as raw materials, and carrying out two-step heating synthesis under the vacuum sealing condition to obtain a product. The nickel disulfide powder synthesized by the method has high purity (more than or equal to 99 percent) and fine particle size (0.074 mm), and can be synthesized in batch, and high-purity iron disulfide and high-purity cobalt disulfide powder can be synthesized by the method.
Description
The present invention relates to a kind of is raw material with the simple substance powder, is synthesized into method high-purity, the particulate NiS 2 powder through two step high temperature.
High-purity NiS 2 powder can improve its electric property as the additive for electrode of lithium/iron disulfide thermobattery, causes people's extensive attention in recent years.The synthetic method of bibliographical information mainly contained in the past: (1) is raw material with nickel powder and SULPHUR POWDER, in high-tension unit, in 6.5 * 10
5KPa heats under 800～1200 ℃ the condition and synthesized in 1～2 hour, and this condition is very harsh, is difficult to realize.(2) single nickel salt being heated to 227 ℃ in the hydrogen sulfide air-flow synthesizes.This method synthetic product crystallinity is poor, and the easy contaminate environment of hydrogen sulfide.
Purpose of the present invention is exactly in order to overcome the shortcoming of aforesaid method, and the method for a kind of not only safety but also the easy high-purity curing nickel of synthetic is provided.
The objective of the invention is to realize by following scheme.
The synthetic method of high-purity NiS 2 powder is characterized in that:
The first step, with high purity elemental nickel powder and SULPHUR POWDER (consumption of SULPHUR POWDER is 1.01～2.0 times of theoretical amount) mixing by a certain percentage, put into quartz glass tube, vacuum condition lower seal at 0.001～0.1Pa, place in the retort furnace then, in 200～700 ℃ of scopes, kept 72～144 hours, be cooled to room temperature, obtain crude product;
In second step, behind crude product grinding, the 0.0074mm that sieves, be reentered in the quartz glass tube, vacuum condition lower seal in 0.001～0.1Pa places in the retort furnace, keeps 72～144 hours in 200～700 ℃ of scopes, be cooled to room temperature, promptly obtain high-purity NiS 2 powder;
Method of the present invention is compared with other method of bibliographical information, and have following characteristics: synthesis temperature is low, and security is good, and easy handling is the method that a kind of more satisfactory batch synthesizes high-purity NiS 2 powder.
Below in conjunction with example method of the present invention is further described.
Example 1 restrains high-purity nickel powder (〉=99.5%) 3.3 grams and specpure SULPHUR POWDER 7.2 in (making excessive 2 times of the SULPHUR POWDER) quartz glass tubes of packing into, be evacuated to 0.001Pa, sealing with this understanding, then quartz glass tube is put into retort furnace, be warmed up to 600 ℃, constant temperature 72 hours, be cooled to room temperature, extract abrasive lapping, the 0.074mm that sieves (200 order), the extracting screen underflow material is packed in another quartz glass tube, in the vacuum condition lower seal of 0.001Pa, put into retort furnace once more and be warming up to 600 ℃, constant temperature 72 hours, promptly obtain NiS 2 powder 6.6 grams, purity is greater than 99%.
Example 2 is according in example 1 same material and step, add nickel powder 176.13 grams and 211.6 gram SULPHUR POWDER (excessive 1.1 times), at the vacuum condition lower seal of 0.1Pa in quartz glass tube, heat temperature raising to 500 ℃ then, constant temperature 72 hours, after cooling off, grinding, sieve, under same vacuum condition, be sealed in again in the silica tube, be warming up to 500 ℃, constant temperature 144 hours, obtain NiS 2 powder 382 grams, purity is greater than 99%.
Example 3 is according in example 1 same material and step, add nickel powder 200 grams and 232 gram SULPHUR POWDER (excessive 1.06 times), at the vacuum condition lower seal of 0.001Pa in quartz glass tube, heat temperature raising to 600 ℃ then, constant temperature 96 hours, cool off, grind, sieve behind the 0.074mm, screen underflow is sealed in the silica tube under same vacuum condition again, is warming up to 600 ℃, constant temperature 72 hours, obtain NiS 2 powder 413 grams, purity is greater than 99%.
Claims (3)
1, a kind of synthetic method of high-purity NiS 2 powder, its inventive features is:
(1). the first step, with high purity elemental nickel powder and SULPHUR POWDER (consumption of SULPHUR POWDER is 1.01～2.0 times of theoretical amount) mixing by a certain percentage, put into quartz glass tube, vacuum condition lower seal at 0.001～0.1Pa, place in the retort furnace then, in 200～700 ℃ of scopes, kept 72～144 hours, be cooled to room temperature, obtain crude product;
(2). in second step, behind crude product grinding, the 0.0074mm that sieves, be reentered in the quartz glass tube, vacuum condition lower seal in 0.001～0.1Pa places in the retort furnace, keeps 72～144 hours in 200～700 ℃ of scopes, be cooled to room temperature, promptly obtain the high-purity NiS 2 powder product;
2, method according to claim 1 is characterized in that: during the first step was synthetic, the optimum amount of SULPHUR POWDER was 1.06 times of theoretical amount, and optimum temperature range is 500～600 ℃;
3, method according to claim 1 is characterized in that: during second step was synthetic, optimum temperature range was 500～600 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99109781A CN1073969C (en) | 1999-07-15 | 1999-07-15 | Synthesis method of high-purity nickel disulfide powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99109781A CN1073969C (en) | 1999-07-15 | 1999-07-15 | Synthesis method of high-purity nickel disulfide powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1240765A true CN1240765A (en) | 2000-01-12 |
| CN1073969C CN1073969C (en) | 2001-10-31 |
Family
ID=5274149
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN99109781A Expired - Fee Related CN1073969C (en) | 1999-07-15 | 1999-07-15 | Synthesis method of high-purity nickel disulfide powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1073969C (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102020320A (en) * | 2010-12-31 | 2011-04-20 | 桂林电子科技大学 | Method for compounding cobalt disulfide |
| CN102633309A (en) * | 2012-01-13 | 2012-08-15 | 沈阳理工大学 | Hydrothermal preparation method for NiS2 with controllable shape |
| CN102751489A (en) * | 2012-06-29 | 2012-10-24 | 上海交通大学 | Method for preparing anode material of lithium ion battery |
| CN104835958A (en) * | 2014-03-27 | 2015-08-12 | 北汽福田汽车股份有限公司 | Preparation method and application of NiS hydrogen storage material |
| CN105680024A (en) * | 2016-04-13 | 2016-06-15 | 扬州大学 | Preparing method for lithium ion battery negative material FeS/CPAN |
| CN107799769A (en) * | 2017-02-20 | 2018-03-13 | 湖南大学 | A kind of nanometer curing nickel material and its preparation method and application |
| CN110803723A (en) * | 2019-12-03 | 2020-02-18 | 兰州理工大学 | Solid-phase synthesis method of high-purity nickel disulfide nanospheres |
| CN113501550A (en) * | 2021-06-25 | 2021-10-15 | 中南大学 | Method for preparing core-shell composite sulfide material by two-step method |
| CN114149035A (en) * | 2021-11-30 | 2022-03-08 | 湖南大学 | Low-temperature synthesis high-specific-capacity NiS2Method for producing powder |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4547347A (en) * | 1983-12-02 | 1985-10-15 | Amax Inc. | Granulometric control of nickel sulfide precipitate |
| JPS60260403A (en) * | 1984-06-04 | 1985-12-23 | Nishimura Watanabe Chiyuushiyutsu Kenkyusho:Kk | Manufacture of metallic sulfide |
| JPH01317105A (en) * | 1988-06-14 | 1989-12-21 | Mitsui Toatsu Chem Inc | Production of metal sulfide |
| FR2657599B1 (en) * | 1990-01-30 | 1992-04-03 | Loire Atlantique Procedes Chim | PROCESS FOR THE PREPARATION OF BINARY SULFUR COMPOUNDS. |
-
1999
- 1999-07-15 CN CN99109781A patent/CN1073969C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102020320A (en) * | 2010-12-31 | 2011-04-20 | 桂林电子科技大学 | Method for compounding cobalt disulfide |
| CN102020320B (en) * | 2010-12-31 | 2012-08-01 | 桂林电子科技大学 | Method for compounding cobalt disulfide |
| CN102633309A (en) * | 2012-01-13 | 2012-08-15 | 沈阳理工大学 | Hydrothermal preparation method for NiS2 with controllable shape |
| CN102751489A (en) * | 2012-06-29 | 2012-10-24 | 上海交通大学 | Method for preparing anode material of lithium ion battery |
| CN104835958A (en) * | 2014-03-27 | 2015-08-12 | 北汽福田汽车股份有限公司 | Preparation method and application of NiS hydrogen storage material |
| CN105680024A (en) * | 2016-04-13 | 2016-06-15 | 扬州大学 | Preparing method for lithium ion battery negative material FeS/CPAN |
| CN107799769A (en) * | 2017-02-20 | 2018-03-13 | 湖南大学 | A kind of nanometer curing nickel material and its preparation method and application |
| CN110803723A (en) * | 2019-12-03 | 2020-02-18 | 兰州理工大学 | Solid-phase synthesis method of high-purity nickel disulfide nanospheres |
| CN113501550A (en) * | 2021-06-25 | 2021-10-15 | 中南大学 | Method for preparing core-shell composite sulfide material by two-step method |
| CN113501550B (en) * | 2021-06-25 | 2022-08-30 | 中南大学 | Method for preparing core-shell composite sulfide material by two-step method |
| CN114149035A (en) * | 2021-11-30 | 2022-03-08 | 湖南大学 | Low-temperature synthesis high-specific-capacity NiS2Method for producing powder |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1073969C (en) | 2001-10-31 |
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Address after: No. 88 South West Fourth Ring Road (Park), Beijing, Fengtai District Patentee after: Beijing Easpring Material Technology Co., Ltd. Address before: No. 88 South West Fourth Ring Road (Park), Beijing, Fengtai District Patentee before: Dangsheng Material Science & Technology Co., Ltd., Beijing |
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Granted publication date: 20011031 Termination date: 20130715 |