CN101138793A - Nanometer powdered iron producing technique - Google Patents
Nanometer powdered iron producing technique Download PDFInfo
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- CN101138793A CN101138793A CNA2006100374363A CN200610037436A CN101138793A CN 101138793 A CN101138793 A CN 101138793A CN A2006100374363 A CNA2006100374363 A CN A2006100374363A CN 200610037436 A CN200610037436 A CN 200610037436A CN 101138793 A CN101138793 A CN 101138793A
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Abstract
The present invention relates to technology of manufacturing nanometer iron powder, which is characterized in that nitrogen of 99.9 per cent purity is preheated in a preheater 1; carbonyl iron steam is mixed with the nitrogen in a mixing channel 2; preheated nitrogen enters a resolver 3 through a pipe and meets the carbonyl iron steam that enters the resolver through a nozzle of the resolver at a top of the resolver; the gas motioned-above has decomposition reaction: Fe(CO)<SUB>5</SUB>is equal to Fe+5CO; heat treatment is practiced for the powder from the decomposition reaction by controlling heating temperature of heating section of airflow resolver to make the powder have good physical property; after airflow classification for the treated powder is completed, coarse particles falls down into a powder-collecting section 6 and most nepheloid powder enters a cooler 5 together with air flow, mixes with cool nitrogen and cools. The cooled powder enters the powder-collecting section 6 and is separated from the gas, and the nanometer carbonyl iron powder is obtained. The gas enters an incinerator 7 after being treated by the powder-collecting section and is discharged after being sterilized.
Description
Affiliated technical field
The invention belongs to a kind of reparation technology of nanometer iron powder.
Background technology
In the present domestic and foreign literature of the reparation technology of nanometer iron powder more report is arranged, majority is mechanical crushing or chemical precipitation method production, since the character of its technology determined the iron powder of producing exist particle inhomogeneous, contain shortcoming such as salt impurity, so do not satisfy the requirement of many industries.
Summary of the invention
Purpose of the present invention is produced the nanometer carbonyl iron dust exactly.
The reparation technology of nanometer iron powder of the present invention mainly is to adopt pure inert gas to make thermal source, produces nano grade iron powder in decomposer.
Purity is that 99.9% nitrogen carries out preheating in preheater, carbonyl iron steam carries out proportioning with nitrogen in mixing channel mixes, the nitrogen that is preheated enters decomposer by pipeline, meets at the decomposer top with the carbonyl iron steam that enters through the decomposer nozzle, produces decomposition reaction:
Fe(CO)
5＝＝Fe+5CO
React the bringing-up section of the powder of generation,, the powder that forms is heat-treated the powder physical property that makes its acquisition desirable by the temperature of control heating with the air-flow decomposer.Treated powder is through behind the air current classifying, coarse granule falls into Ji Fencang, most of vaporific powder enters in the cooler with air-flow and mixes cooling fast with the cold nitrogen that enters, and cooled powder enters Ji Fencang to be separated with gas, can obtain the carbonyl iron dust of nanometer.Gas enters incinerator sterilization back discharging through receiving after the powder device is handled.
The powder of output has extremely strong activity, so must carry out Passivation Treatment, sieves at the inert gas that is mixed with 0.1% oxygen, makes its surface form diaphragm.Help storing, transport and use.
It is a lot of to influence powder size size factor, as the concentration of carbonyl iron steam, nitrogen preheat temperature, nitrogen flow etc.Wherein carbonyl iron steam concentration is the factor that directly influences powder size size most critical.
The influence of carbonyl iron steam concentration.Along with the reduction of carbonyl iron steam, powder size attenuates, as shown in Figure 2.
Nitrogen gives hot Temperature Influence.The height that gives the hot nitrogen temperature to the influence of powder size as shown in Figure 3.As can be seen along with the rising of giving hot temperature, the specific area of powder increases by table, and promptly granularity attenuates, and behind certain value, temperature raises again then more heat surplus, and the powder collision probability is increased, and the nuclear coarsening rate is accelerated, thus the powder size chap.
Give the influence of hot nitrogen flow.The flow that is heated nitrogen is that what to influence granule size is again a principal element.As shown in Figure 4.Found out that by figure along with the increase of giving the hot nitrogen flow, specific surface area is long-pending to become big, granularity attenuates, until limiting value occurs.When nitrogen flow during greater than limiting value, too much heat makes the granularity chap of growing up.
Best process conditions are the keys of producing the nanoscale carbonyl iron dust, it is as follows that the present invention controls above-mentioned all technological factors: nitrogen gives 400～600 ℃ of hot temperature, the flow that gives hot nitrogen is 300～600 liters/minute, the nitrogen flow that is used for the carbonyl iron steam proportioning is 100～300 liters/minute, the flow of carbonyl iron steam is 5～10 liters/minute, total nitrogen: carbonyl iron steam=90-100: 1, air in the passivation gas: nitrogen=1: 20-30 produces the granularity of powder and specific area and concerns that available following relational expression represents:
D＝55.5-0.55Sg
In the formula: D----particle mean size (nm)
Sg----specific area (m
2/ g)
Description of drawings
Fig. 1 is nanometer carbonyl iron dust technological process of production figure.
1 for nitrogen gives hot stove, and 2 is the mixing channel that nitrogen, carbonyl iron steam mix, and 3 is decomposer, and 4 is meal Ji Fencang, and 5 is cooler, and 6 is fine powder Ji Fencang, and 7 is incinerator
Fig. 2 is the influence variation diagram of carbonyl iron steam concentration to granularity.
Fig. 3 is the influence variation diagram of nitrogen temperature to granularity.
Fig. 4 is the influence variation diagram of nitrogen flow to granularity.
Fig. 5 is that two groups of technological parameters and result thereof contrast tabulation figure.
The specific embodiment
Purity is that 99.9% nitrogen carries out preheating in preheater 1, carbonyl iron steam carries out proportioning with nitrogen in mixing channel 2 mixes, the nitrogen that is preheated enters decomposer 3 by pipeline, meets at the decomposer top with the carbonyl iron steam that enters through the decomposer nozzle, produces decomposition reaction:
Fe(CO)
5＝＝Fe+5CO
React the bringing-up section of the powder of generation,, the powder that forms is heat-treated the powder physical property that makes its acquisition desirable by the temperature of control heating with the air-flow decomposer.Treated powder is through behind the air current classifying, coarse granule falls into collection powder storehouse 4, most of vaporific powder enters in the cooler 5 with air-flow and mixes cooling fast with the cold nitrogen that enters, and cooled powder enters collection powder storehouse 6 to be separated with gas, can obtain the carbonyl iron dust of nanometer.Gas enters incinerator 7 sterilization back dischargings through receiving after the powder device is handled.
The powder of output has extremely strong activity, so must carry out Passivation Treatment, sieves at the inert gas that is mixed with 0.1% oxygen, makes its surface form diaphragm.Help storing, transport and use.
It is a lot of to influence powder size size factor, as the concentration of carbonyl iron steam, nitrogen preheat temperature, nitrogen flow etc.Wherein carbonyl iron steam concentration is the factor that directly influences powder size size most critical.
According to above-mentioned technological process, and, adopted following technological parameter, thereby made nano level carbonyl iron dust according to determined technological parameter.Fig. 5 has enumerated two groups of technological parameters and result thereof.
Claims (9)
1. the reparation technology of nanometer iron powder, it is characterized in that: purity is that 99.9% nitrogen carries out preheating in preheater 1, carbonyl iron steam carries out proportioning with nitrogen in mixing channel 2 mixes, the nitrogen that is preheated enters decomposer 3 by pipeline, meet at the decomposer top with the carbonyl iron steam that enters through the decomposer nozzle, produce decomposition reaction:
Fe(CO)
5＝＝Fe+5CO
React the bringing-up section of the powder of generation,, the powder that forms is heat-treated the powder physical property that makes its acquisition desirable by the temperature of control heating with the air-flow decomposer.Treated powder is through behind the air current classifying, coarse granule falls into collection powder storehouse 4, most of vaporific powder enters in the cooler 5 with air-flow and mixes cooling fast with the cold nitrogen that enters, and cooled powder enters collection powder storehouse 6 to be separated with gas, can obtain the carbonyl iron dust of nanometer; Gas enters incinerator 7 sterilization back dischargings through receiving after the powder device is handled.
2. method according to claim 1 is characterized in that the powder of output has extremely strong activity, so must carry out Passivation Treatment, sieves at the inert gas that is mixed with 0.1% oxygen, makes its surface form diaphragm; Help storing, transport and use.
3.3, method according to claim 1, it is characterized in that nitrogen enters decomposer before, gas heating stove must be arranged.
4. according to claim 1 and 2 described methods, the preheat temperature temperature that it is characterized in that nitrogen is 400-600 ℃.
5. according to claim 1,2 and 3 described methods, the flow that it is characterized in that pre-hot nitrogen is 300～600 liters/minute.
6. method according to claim 1, the nitrogen flow that it is characterized in that the carbonyl iron steam proportioning is 100～300 liters/minute.
7. according to claim 1 and 5 described methods, the flow that it is characterized in that carbonyl iron steam is 5～10 liters/minute.
8. according to claim 1,4 and 6 described methods, it is characterized in that total nitrogen: carbonyl iron steam=90-100: 1.
9. method according to claim 1 is characterized in that air in the passivation gas: nitrogen=1: 20-30.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006100374363A CN101138793A (en) | 2006-09-04 | 2006-09-04 | Nanometer powdered iron producing technique |
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|---|---|---|---|
| CNA2006100374363A CN101138793A (en) | 2006-09-04 | 2006-09-04 | Nanometer powdered iron producing technique |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102689008A (en) * | 2011-03-23 | 2012-09-26 | 杰富意钢铁株式会社 | Method of finish heat treatment of iron powder and apparatus for finish heat treatment |
| CN102839394A (en) * | 2012-09-17 | 2012-12-26 | 哈尔滨工业大学 | Method for rapidly preparing tree-like nano-iron with multi-level structure |
| CN104384521A (en) * | 2014-08-28 | 2015-03-04 | 江苏艾科勒科技有限公司 | Quick controllable nano-iron active material preparation device |
| CN104551013A (en) * | 2014-12-07 | 2015-04-29 | 金川集团股份有限公司 | Method for controlling particle size of carbonyl iron powder during decomposition process |
| CN104588680A (en) * | 2014-12-07 | 2015-05-06 | 金川集团股份有限公司 | Carbonyl iron decomposition method capable of controlling oxygen content in iron powder |
| CN105945303A (en) * | 2016-05-17 | 2016-09-21 | 西北师范大学 | Preparing method of nano alpha-Fe metal powder |
| CN106623957A (en) * | 2016-11-30 | 2017-05-10 | 江永斌 | Nano particle grower capable of realizing continuous mass production of superfine nanoscale metal particles |
| CN107225233A (en) * | 2017-07-17 | 2017-10-03 | 金川集团股份有限公司 | It is a kind of that the device and method that powder is passivated is produced to carbonyl process |
| CN114346533A (en) * | 2022-01-05 | 2022-04-15 | 重庆工商大学 | Track regulation and control device for welding automobile parts |
| CN115785927A (en) * | 2021-09-09 | 2023-03-14 | 中国石油天然气集团有限公司 | High-stability micro-nano spherical weighting agent and preparation and application thereof |
-
2006
- 2006-09-04 CN CNA2006100374363A patent/CN101138793A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102689008A (en) * | 2011-03-23 | 2012-09-26 | 杰富意钢铁株式会社 | Method of finish heat treatment of iron powder and apparatus for finish heat treatment |
| CN102839394A (en) * | 2012-09-17 | 2012-12-26 | 哈尔滨工业大学 | Method for rapidly preparing tree-like nano-iron with multi-level structure |
| CN102839394B (en) * | 2012-09-17 | 2014-10-15 | 哈尔滨工业大学 | Method for rapidly preparing tree-like nano-iron with multi-level structure |
| CN104384521A (en) * | 2014-08-28 | 2015-03-04 | 江苏艾科勒科技有限公司 | Quick controllable nano-iron active material preparation device |
| CN104551013A (en) * | 2014-12-07 | 2015-04-29 | 金川集团股份有限公司 | Method for controlling particle size of carbonyl iron powder during decomposition process |
| CN104588680A (en) * | 2014-12-07 | 2015-05-06 | 金川集团股份有限公司 | Carbonyl iron decomposition method capable of controlling oxygen content in iron powder |
| CN105945303A (en) * | 2016-05-17 | 2016-09-21 | 西北师范大学 | Preparing method of nano alpha-Fe metal powder |
| CN106623957A (en) * | 2016-11-30 | 2017-05-10 | 江永斌 | Nano particle grower capable of realizing continuous mass production of superfine nanoscale metal particles |
| CN107225233A (en) * | 2017-07-17 | 2017-10-03 | 金川集团股份有限公司 | It is a kind of that the device and method that powder is passivated is produced to carbonyl process |
| CN107225233B (en) * | 2017-07-17 | 2019-09-13 | 金川集团股份有限公司 | The device and method that a kind of pair of carbonyl process production powder is passivated |
| CN115785927A (en) * | 2021-09-09 | 2023-03-14 | 中国石油天然气集团有限公司 | High-stability micro-nano spherical weighting agent and preparation and application thereof |
| CN115785927B (en) * | 2021-09-09 | 2024-01-23 | 中国石油天然气集团有限公司 | High-stability micro-nano spherical weighting agent and preparation and application thereof |
| CN114346533A (en) * | 2022-01-05 | 2022-04-15 | 重庆工商大学 | Track regulation and control device for welding automobile parts |
| CN114346533B (en) * | 2022-01-05 | 2023-09-01 | 重庆工商大学 | Track regulation and control device for welding automobile parts |
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