CN1031400A - The production method of hypoxemia chromium powder - Google Patents
The production method of hypoxemia chromium powder Download PDFInfo
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A kind ofly reduce deoxidation and produce the production method of hypoxemia chromium powder.With the electrolytic chromium powder is raw material, is heating thermal source and reductive agent with the hydrogen plasma.The working gas of plasma body and the carrier gas of raw material are hydrogen.The granularity of electrolytic chromium powder is the 3-60 micron.The reduction deoxidation temperature is 1500 ℃-4000 ℃.Product granularity is less than 200 orders, and oxygen level is less than 0.2%, and carbon content is low.Can be used as the raw material of the coated material of sintering metal, wear-and corrosion-resistant, especially can be used as the raw material of mechanical alloying superalloy.This law technology and equipment are simple, and cost is low, and is with short production cycle, but continuous production, treatment capacity is big, and the total yield of chromium powder is up to 99%.
Description
The present invention relates to produce the processing method of hypoxemia chromium powder, a kind of more precisely method of refining of chromium powder reduction deoxidation with the hydrogen plasma method.
Chromium powder is except that being used for superalloy, and also coated material, the evaporating materials on the electronic industry and the preparation as sintering metal, wear-and corrosion-resistant has the additive of the switch contact alloy of resistance of oxidation.What is more important is as the important source material of mechanical alloying superalloy.
The main method of producing chromium powder at present is the aqueous electrolysis with chromic salt, but the oxygen level of electrolytic chromium powder generally very high (0.7-1.0%, weight percentage below do not specialize, and are weight percentage), carbon content does not conform with the requirement of such use yet.In order to obtain chromium powder, must do further refining reduction deoxidation to electrolytic chromium powder as such use.
The reduction method of deoxidation of existing electrolytic chromium powder has following four kinds: (1) high temperature in hydrogen stream is refining; (2) heating under vacuum degassing deoxidation; (3) iodate is refining; (4) zone melting.Except first method, other three kinds of methods all owing to the processing cost height, treatment capacity is little and purify after product be not powdery and not being used widely.
US4,148,628 have proposed a kind of processing method of producing chromium metal.With chromium sesquioxide and carbon black, graphite and refinery coke is raw material, with any fine powder that is mixed and made in chromium sesquioxide and carbon black, graphite and the refinery coke, add tackiness agent again and make the particle of big or small average out to 0.01-3.0 millimeter, the preferably particle of 0.01-1.0 millimeter; With hydrogen, methane or their mixture, it is sent in the plasma body, more than 1200 ℃ chromium sesquioxide is being reduced into chromium metal; The working gas of plasma body is any mixed gas in argon or argon-hydrogen, argon-methane and the hydrogen-methane; The chromium metal that generates contains the oxygen of 0.5-3.0% and the carbon of 0.5-3.0%, therefore needs further refining.Refining is carried out with two kinds of methods.First method is that product is worn into powder, adds carbon and tackiness agent is made agglomerate, and agglomerate is put into vacuum oven, maintains the temperature between 1200 °-1500 ℃, and pressure is the 0.1-20 torr, reduces in solid phase; Second method is that this agglomerate is placed in the plasma heating furnace with in the water-cooled container, heats agglomerate with plasma flame under protective atmosphere, reduces under molten state.The product that two kinds of method of refining obtain also needs carbonization treatment, promptly under the condition that does not have hydrogen to exist in plasma heating furnace heating carry out oxidation and decarbonization.
A.H.Sully(" CHROMIUM " second edition, P67,1967, London Butterworths) use hydrogen reduction at 1500 ℃, to remove the oxygen in the chromium powder.The particle diameter of raw material chromium powder is advisable between the 152-635 micron.If use thinner chromium powder, can cause the sintering of chromium powder, influence the diffusion of hydrogen, also can not get powder-like product simultaneously; If the particle of raw material too in big (greater than 1000 microns) or the boat thickness of chromium powder layer surpass 1 millimeter, all deoxidations well.
(Journal of the institute of metal such as H.T.Greenaway, Vol.83,121-125, heat with high frequency furnace when 1954-55) removing oxygen in the chromium powder with hydrogen, can rapid heating and cooling, the generation of chromium powder re-oxidation reaction in the time that so low temperature can being reduced, but also there is the restricted problem of raw material particle size.
(ε lectrochem.Soc. such as J.Kroll, 97,258-264,1950) be raw material with 65 purpose electrolytic chromium powder (contain 1% chromium sesquioxide, promptly contain oxygen 0.31%), use the hydrogen reduction deoxidation, the reduction deoxidation temperature is 1000 ℃, for up to three days, the oxygen level of its product was 0.063%, and product partially sinters.
In a word, the method that electrolytic chromium powder is led to the hydrogen reduction deoxygenation refining with vertical or horizontal electric heating tube furnace, high frequency furnace heating takes length, treatment capacity is little, efficient is low; At high temperature the product chromium powder easily produces serious sintering; And chromium powder particle surface fusing under the high temperature, reductive agent hydrogen is difficult for infiltrating its inside.In the deoxidation of high temperature reaction zone hydrogen reducing, and at the cold zone reaction product water with product chromium powder oxidation again, promptly have the danger reoxidize; Can not produce less than 200 purposes and contain oxygen, the chromium powder that meets such use that carbon containing is low; At high temperature the reactor quartz material can be SiO by hydrogen reduction, the polluted product chromium powder.
US4, the method for refining of 148,628 chromium needs deoxidation, two processing steps of decarburization, complex process can not continuous production, the cost height, though the refining chromium powder oxygen level of producing is low, the carbon content height, can not obtain meeting such use less than 200 purpose chromium powders.
Purpose of the present invention, the first work out a kind of production method of hypoxemia chromium powder.The hypoxemia chromium powder of producing also can be used as the coated material of sintering metal, wear-and corrosion-resistant except that being used for superalloy; The additive of the switch contact alloy that has resistance of oxidation as the evaporating materials on the electronic industry and preparation particularly importantly can be used as mechanical alloying superalloy raw material; It two is that this production method technology is simple, cost is low, and product cut size is less than 200 orders, and the carbon of product, oxygen level can meet the requirement of such use; It three is that ultra-fine chromium powder can access alligatoring and deoxidation.
The present invention is a kind of production method of hypoxemia chromium powder, is raw material with the electrolytic chromium powder, with hydrogen plasma as heating thermal source and reductive agent; Hydrogen plasma effusive direction is from bottom to top, and the feedstock direction of electrolytic chromium powder is from the top down, falls into the hydrogen plasma high-temperature zone; The plasma body working gas is a hydrogen, and carrying the carrier gas of electrolytic chromium powder is hydrogen; The granularity of electrolytic chromium powder is 3 microns-60 microns, and the temperature of the hydrogen plasma high-temperature zone of reduction deoxidation electrolytic chromium powder is 1500 °-4000 ℃.
In order to make the hydrogen plasma fluidic operation be in steady state, the flow of plasma body working gas hydrogen be controlled at 40 liters-70 liters/be divided into, flow is less than 40 liters/minute, plasma gun is easy to burn; Greater than 70 liters/minute, the part material electrolytic chromium powder can be blown away, and the plasma arc instability, is easily blown out.
The flow of the carrier gas hydrogen of transferring raw material electrolytic chromium powder with 27 liters-31 liters/be divided into.
Globule size as the electrolytic chromium powder of raw material has bigger influence to deoxidation effect.The chromium powder granularity is unfavorable for deoxidation greatly, because granularity is big, hydrogen is then long to the time that intraparticle diffusion needs, and the time that particle stays in the high-temperature zone is shorter, has therefore reduced deoxidation effect.From table 1, can be clear that the influence of globule size to deoxidation.
Table 1. raw material electrolytic chromium powder globule size is to the influence of deoxidation
Granularity as the electrolytic chromium powder of raw material is 3 microns-60 microns, is good with 4 microns-8 microns; Along with diminishing of electrolytic chromium powder granularity, the deoxidation rate increases; But during less than 3 microns, make reinforced generation difficulty, and raw material generating gasification; Greater than 60 microns, the raw material lowering speed increases, and makes it in high-temperature zone shortening residence time, and the diffusion time minimizing of hydrogen in particle is unfavorable for deoxidation.
Oxygen level in the raw material electrolytic chromium powder is high more, and the deoxidation rate is high more; With oxygen level more than 0.2%-3% for well, be again that 0.25%-0.9% is better with the oxygen level.
The raw material electrolytic chromium powder is very short residence time in the plasma high-temperature district, is generally 5-15 second.So, when raw material electrolytic chromium powder oxygen level is high, need just can make oxygen level reach requirement, but each recovery time is very short through repeatedly reducing deoxidation repeatedly.Along with the increase of reduction deoxidation number of times, the oxygen level in the chromium powder also reduces gradually.Increase reduction deoxidation number of times and be equivalent to increase the residence time of chromium powder in the high-temperature zone.When feed oxygen content was not high, once reduction also can obtain oxygen level less than 0.2% product.The raw material electrolytic chromium powder is repeatedly reduced the effect of deoxidation and is listed in table 2.
Table 2. raw material electrolytic chromium powder is repeatedly reduced deoxidation effect
Usually the raw material electrolytic chromium powder is reduced deoxidation repeatedly in 5 times, but also can be greater than 5 times.The raw material electrolytic chromium powder need be reduced the deoxidation how many times repeatedly, decide on the various factorss such as oxygen level, raw material electrolytic chromium powder particulate size and the desired oxygen level of product of raw material electrolytic chromium powder.
Feed rate has certain influence to the reduction deoxidation.Under same power, along with the increase of feed rate, the deoxidation rate also increases, but certain limit is arranged.Under power used in the present invention, feed rate is advisable with 15 grams-90 Grams Per Minutes.Less than 15 Grams Per Minutes, the yielding poorly of product, raw material is gasificated into ultrafine powder easily; Greater than 90 Grams Per Minutes, the temperature of reaction of reduction deoxidation is reduced, the deoxidation rate reduces.
The temperature of the hydrogen plasma high-temperature zone of reduction deoxidation electrolytic chromium powder is 1500 °-4000 ℃, but be good (with spectral line absolute intensity method mensuration temperature) with 1800 °-2300 ℃.
In order to reduce the oxygen level in the product, employed hydrogen must be purified, i.e. deoxidation dehydration.Method of purification is to carry out one-level with silica gel successively to dewater, and carries out secondary with molecular sieve and dewaters, and with No. 105 catalyzer deoxygenations, carries out third class de-watering with molecular sieve again, finally obtains needed pure hydrogen.
Advantage of the present invention is:
1. because using plasma high temperature dilute phase reduction, avoided the sintering of chromium powder, product all can pass through 200 mesh standard sieves, and the oxygen level of product is less than 0.2%, minimumly reaches 0.13%.This law is deoxidation effectively, and can also denitrogenation, decarburization and other lower boiling metallic impurity, for example, Al, Pb, Mn etc., the content of Cu impurity also decreases, and the results are shown in Table 3, table 4.Therefore the product produced of present method meets the requirement of such use fully, except that can be used for superalloy, can also be as sintering metal, wear-resisting, anti-corrosion coated material, can be used as the additive that preparation has resistance of oxidation switch contact alloy, particularly importantly can be used as the raw material of mechanical alloying superalloy.
The variation of nitrogen, carbon content in the chromium powder before and after table 3. is handled
*
The variation of metallic impurity before and after the deoxidation of table 4. chromium powder
*
* carbon high-frequency combustion infrared absorption method; Nitrogen is measured with the Kai Shi distillation method, down together
The * spectroscopic analysis
2. technology of the present invention and equipment are all simple, mainly use hydrogen, and recyclable repeated use, and product cost is low, but continuous production, output is big, and is with short production cycle, and the total yield height of chromium powder can reach 99%.
3. owing to the internal heating mode of using plasma, the plasma reaction wall carries out water-cooled, does not therefore have the problem of the material of reactor to product contamination.
4. in the reduction deoxidation process, can be separated in the ultrafine powder that forms in the reaction process automatically, ultrafine powder can be returned.
5. because the using plasma heating heats up and the temperature fall time weak point, shortened the operational cycle; The plasma high-temperature district because the product chromium powder speeds away can access rapid cooling, the chromium powder danger of oxidation again when having avoided cooling.
6. suitably alligatoring of the chromium powder produced of this law has improved flowability and loose specific weight, particle shape subglobular or slynessization.
Accompanying drawing, the plasma reactor sectional view of using in the processing method of the present invention.
In the accompanying drawing, plasma reactor (1) has water-cooled stainless steel wall (2); At the top of plasma reactor (1) feed-pipe (7) is housed, feed-pipe (7) is connected with plasma reactor (1) with flange (3); Side wall upper part at plasma reactor (1) is equipped with tail gas outlet (8) and water-in (9) and water outlet (10), in its bottom discharge port (4) and plasma gun (5) is housed; (6) be the hydrogen flame passes.
The raw material electrolytic chromium powder is placed in the electric and magnetic oscillation powder feeder, feed carrier gas H
2, start powder feeder, make raw material pass through in the plasma high-temperature district that feed-pipe (7) enters the hydrogen flame passes (6) in the plasma reactor (1) chromium sesquioxide in the chromium powder to be reduced rapidly, some metallic impurity is removed in deoxidation, denitrogenation, decarburization; The raw material electrolytic chromium powder is stayed 5-15 second in the hydrogen plasma high-temperature zone, and plasma high-temperature district then speeds away; Product enters in the collector by discharge port (4), tail gas emptying after fly-ash separator trap filter ultrafine powder.
Arc current is controlled at (arc voltage 80V-150V) between the 150A-250A usually.
More specifically describe the present invention with following indefiniteness embodiment, protection scope of the present invention is not subjected to the qualification of these embodiment.
Equipment used is (power 20-40 kilowatt of plasma generator power supply and a spray gun, Jiujiang plasma spraying equipment factory produces), plasma reactor is the outer water cooled reactor of stainless steel, fly-ash separator is DC-2 unit fly-ash separator (Beijing motorbus repair plant), electric and magnetic oscillation powder feeder (Xianfeng Electric Motor Factory); Used hydrogen must carry out one-level through silica gel (Beijing Chemical Plant) and dewater, carrying out secondary with 5A molecular sieve (the Dalian Chemistry and Physics Institute) dewaters, with No. 105 catalyzer (the Dalian Chemistry and Physics Institute) deoxygenation, carry out third class de-watering with the 5A molecular sieve again, the pure hydrogen dew point of gained is-65 ℃, and oxygen level is less than 20ppm.
Raw material is-300 order electrolytic chromium powder (Shanghai 901 factories, oxygen level 0.784%-0.9%).Drying adds in the electric and magnetic oscillation powder feeder, with carrier gas hydrogen (29 liters/minute of flows) the raw material electrolytic chromium powder is sent into hydrogen plasma high-temperature zone in the hydrogen flame passes through feed-pipe, temperature is 1800 °-2300 ℃, but there is a small amount of feed particles also can fall into 1000 °-1500 ℃ and 1500 °-1800 ℃ and 2300 °-4000 ℃ warm area, the flow of working gas hydrogen is 68 liters/minute, arc voltage 140V, arc current 200A, feed rate is 60 Grams Per Minutes, product oxygen level 0.426%, deoxidation rate are 45.6%.Be raw material with this product again, through three reduction deoxidations repeatedly, the oxygen level of the finished product chromium powder is 0.198%, and chromium powder all can pass through 200 mesh standard sieves.
Equipment and schedule of operation, condition are just reduced deoxidation once substantially with embodiment 1, the operational condition different with embodiment 1 and the results are shown in table 5.
Operational condition and result that table 5. and embodiment 1 are different
Equipment and schedule of operation, condition are just reduced deoxidation once substantially with embodiment 1, the operational condition different with embodiment 1 and the results are shown in table 6.
Operational condition and result that table 6. and embodiment 1 are different
Equipment and schedule of operation, condition are just reduced deoxidation once substantially with embodiment 1, the operational condition different with embodiment 1 and the results are shown in table 7.
Operational condition and result that table 7. and embodiment 1 are different
Equipment and schedule of operation, condition are just reduced deoxidation once substantially with embodiment 1, the operational condition different with embodiment 1 and the results are shown in table 8.
Operational condition and result that table 8. and embodiment 1 are different
Claims (7)
1, a kind of production method of hypoxemia chromium powder is a raw material with the electrolytic chromium powder.Feature of the present invention is:
1) with hydrogen plasma as heating thermal source and reductive agent,
2) hydrogen plasma effusive direction is from bottom to top, and the feedstock direction of electrolytic chromium powder is from the top down, falls into the hydrogen plasma high-temperature zone,
3) carrier gas of the working gas of plasma body and conveying electrolytic chromium powder is hydrogen.
4) granularity of electrolytic chromium powder is 3 microns-60 microns,
5) temperature of hydrogen plasma high-temperature zone is 1500 °-4000 ℃.
2, according to the production method of a kind of hypoxemia chromium powder of claim 1, it is characterized in that the flow of plasma body working gas hydrogen is 40 liters-70 liters/minute, carrying the flow of the carrier gas hydrogen of electrolytic chromium powder is 27 liters-31 liters/minute.
3, according to the production method of a kind of hypoxemia chromium powder of claim 1, it is characterized in that the granularity of raw material electrolytic chromium powder is the 4-8 micron.
According to the production method of a kind of hypoxemia chromium powder of claim 1, it is characterized in that 4, the oxygen level of raw material electrolytic chromium powder is more than 0.2%-3.0%.
5, according to the production method of a kind of hypoxemia chromium powder of claim 4, it is characterized in that the oxygen level of raw material electrolytic chromium powder is 0.25%-0.9%.
According to the production method of a kind of hypoxemia chromium powder of claim 1, it is characterized in that 6, the temperature of hydrogen plasma high-temperature zone of deoxidation chromium powder of reducing is 1800 °-2300 ℃.
7, according to the production method of a kind of hypoxemia chromium powder of claim 1, it is characterized in that, said hydrogen successively through silica gel, molecular sieve dewater, No. 105 catalyzer deoxygenations, molecular sieves dewater.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN87105359.4A CN1004637B (en) | 1987-08-05 | 1987-08-05 | Method for producing low-oxygen chromium powder |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN87105359.4A CN1004637B (en) | 1987-08-05 | 1987-08-05 | Method for producing low-oxygen chromium powder |
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| CN1031400A true CN1031400A (en) | 1989-03-01 |
| CN1004637B CN1004637B (en) | 1989-06-28 |
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| CN87105359.4A Expired CN1004637B (en) | 1987-08-05 | 1987-08-05 | Method for producing low-oxygen chromium powder |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102576603A (en) * | 2010-03-31 | 2012-07-11 | 日东电工株式会社 | Permanent magnet and manufacturing method for permanent magnet |
| CN102808092A (en) * | 2012-09-14 | 2012-12-05 | 苏州晶纯新材料有限公司 | Method for preparing ultra low-oxygen chromium sheets |
| CN102814501A (en) * | 2012-09-14 | 2012-12-12 | 苏州晶纯新材料有限公司 | Preparation method of ultralow-oxygen chromium powder |
| CN102825257A (en) * | 2012-08-21 | 2012-12-19 | 苏州晶纯新材料有限公司 | Method for preparing ultrafine chromium powder |
| CN104070171A (en) * | 2014-06-12 | 2014-10-01 | 陕西斯瑞工业有限责任公司 | Preparation method for superfine chromium powder |
| CN104070172A (en) * | 2014-06-23 | 2014-10-01 | 陕西斯瑞工业有限责任公司 | Method for preparing spherical chromium powder |
| CN105517736A (en) * | 2013-09-02 | 2016-04-20 | 攀时奥地利公司 | Chromium metal powder |
| CN107385240A (en) * | 2017-07-25 | 2017-11-24 | 北京兴荣源科技有限公司 | It is a kind of can mass production electrolysis chromium piece degasification technique |
| CN111531164A (en) * | 2020-04-15 | 2020-08-14 | 河南中钻新材料有限公司 | Method for reducing oxygen and nitrogen contents in chromium powder particles at low cost |
| CN111922350A (en) * | 2020-09-22 | 2020-11-13 | 西安斯瑞先进铜合金科技有限公司 | Preparation method of low-hydrochloric-acid-insoluble metal chromium powder |
| CN112091224A (en) * | 2020-11-11 | 2020-12-18 | 西安斯瑞先进铜合金科技有限公司 | Method for preparing metal chromium powder by ultralow temperature grinding |
-
1987
- 1987-08-05 CN CN87105359.4A patent/CN1004637B/en not_active Expired
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102576603A (en) * | 2010-03-31 | 2012-07-11 | 日东电工株式会社 | Permanent magnet and manufacturing method for permanent magnet |
| CN102825257A (en) * | 2012-08-21 | 2012-12-19 | 苏州晶纯新材料有限公司 | Method for preparing ultrafine chromium powder |
| CN102808092A (en) * | 2012-09-14 | 2012-12-05 | 苏州晶纯新材料有限公司 | Method for preparing ultra low-oxygen chromium sheets |
| CN102814501A (en) * | 2012-09-14 | 2012-12-12 | 苏州晶纯新材料有限公司 | Preparation method of ultralow-oxygen chromium powder |
| CN102808092B (en) * | 2012-09-14 | 2013-09-18 | 苏州晶纯新材料有限公司 | Method for preparing ultra low-oxygen chromium sheets |
| CN102814501B (en) * | 2012-09-14 | 2014-03-26 | 苏州晶纯新材料有限公司 | Preparation method of ultralow-oxygen chromium powder |
| CN105517736A (en) * | 2013-09-02 | 2016-04-20 | 攀时奥地利公司 | Chromium metal powder |
| CN105517736B (en) * | 2013-09-02 | 2019-08-06 | 攀时奥地利公司 | Chromium metal powder and preparation method thereof |
| US11117188B2 (en) | 2013-09-02 | 2021-09-14 | Plansee Se | Chromium metal powder |
| CN104070171A (en) * | 2014-06-12 | 2014-10-01 | 陕西斯瑞工业有限责任公司 | Preparation method for superfine chromium powder |
| CN104070172A (en) * | 2014-06-23 | 2014-10-01 | 陕西斯瑞工业有限责任公司 | Method for preparing spherical chromium powder |
| CN107385240A (en) * | 2017-07-25 | 2017-11-24 | 北京兴荣源科技有限公司 | It is a kind of can mass production electrolysis chromium piece degasification technique |
| CN111531164A (en) * | 2020-04-15 | 2020-08-14 | 河南中钻新材料有限公司 | Method for reducing oxygen and nitrogen contents in chromium powder particles at low cost |
| CN111531164B (en) * | 2020-04-15 | 2022-03-04 | 河南中钻新材料有限公司 | Method for reducing oxygen and nitrogen contents in chromium powder particles at low cost |
| CN111922350A (en) * | 2020-09-22 | 2020-11-13 | 西安斯瑞先进铜合金科技有限公司 | Preparation method of low-hydrochloric-acid-insoluble metal chromium powder |
| CN111922350B (en) * | 2020-09-22 | 2021-01-01 | 西安斯瑞先进铜合金科技有限公司 | Preparation method of low-hydrochloric-acid-insoluble metal chromium powder |
| CN112091224A (en) * | 2020-11-11 | 2020-12-18 | 西安斯瑞先进铜合金科技有限公司 | Method for preparing metal chromium powder by ultralow temperature grinding |
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|---|---|
| CN1004637B (en) | 1989-06-28 |
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