CN1676252A - Method for preparing natural micro alloy iron powder from vanadium-titanium-iron headings by microwave radiation - Google Patents
Method for preparing natural micro alloy iron powder from vanadium-titanium-iron headings by microwave radiation Download PDFInfo
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- CN1676252A CN1676252A CN 200510010766 CN200510010766A CN1676252A CN 1676252 A CN1676252 A CN 1676252A CN 200510010766 CN200510010766 CN 200510010766 CN 200510010766 A CN200510010766 A CN 200510010766A CN 1676252 A CN1676252 A CN 1676252A
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Abstract
The present invention relates to a method for extracting nature microalloy iron powder by utilizing microwave radiation to heat varadium-titanium-iron concentration pellet containing compound additive, said compound additive contains 10-20% of coke, 0-5% of sodium sulfate and 0-5% of iron powder. Said method includes the following steps: controlling pellet drying temperature at 130-150 deg.C for 30-40 min; adding 20%-50% of reductant agent coke, making reduction in microwave oven, reduction temperature is 1100-1300 deg.C and time is 60-120 min, after the pellet is broken, using hydrogen gas with 5-7 H min to make reduction, reduction temperature is 750-850 deg.C and reduction time is 120-240 min. so as to obtain the microallyiron powder whose grain size is less than 180 micrometers.
Description
(1) technical field: metallurgical technology field
(2) background technology
The known technology of producing iron powder with sefstromite concentrate have Liang Diande's " directly also technology the vanadium titano-magnetite ferrotitanium separate and process for extracting vanadium in utilization inquire into " narrated the Soviet Union in (" heavy steel technology " the 3rd phase in 2002) and reported that the sodium salt of interpolation 15% in the sefstromite concentrate was 1050 ℃ of reduction, levigate then, magnetic separation obtain the iron powder of iron content more than 98% and contain TiO
2The rich titanium material of 75-80%; Poland has also reported in succession that with state such as New Zealand reduction grinding separates the result of the test of v-ti magnetite concentrate, but iron, titanium separating effect are undesirable; " tunnel cave-reduction grinding method is produced iron powder used in metallurgy " that Panzhihua mine company adopts Changsha Mining ﹠ Metallurgy Inst to provide, these process conditions are 1150 ℃ of reduction temperatures, recovery time (referring to when the reduction of laboratory employing 400g material) 4h, the total consumption of coke (Jiao/ore deposit) 50-55%; Adopt two choosings of two mills after broken, the primary grinding granularity accounts for 65% less than 75um, the secondary grinding granularity accounts for 55% less than 75um, gravity treatment is all adopted in two sections ore dressings, 800 ℃ of annealing temperatures, temperature retention time 2.5h reflects in commerical test, therefore drawbacks such as this technology refractory consumption rate is big, energy consumption is high, yield rate is low finally are forced to stop production owing to cost is too high; " rotary kiln one reduction grinding method is produced the steely iron powder " that Qiu Guanzhou etc. adopt Central South University to provide in " cooled agglomerated pellet directly reduces " (publishing house of Central South University), these process conditions are 1100 ℃ of reduction temperatures, recovery time 3h, the total consumption of coke (carbon/iron) 68%, adopt two choosings of two mills after broken, the primary grinding granularity is for to account for 99% less than 75um, the secondary grinding granularity is for to account for 96% less than 75um, magnetic separation is all adopted in two sections ore dressings, and the weakness of this technology maximum is, based on the reason of ring formation of rotary kiln, reduction temperature is not higher than 1100 ℃, thereby cause under the routine heating, the iron grain growth is undesirable, and consequently product granularity is thin, TFe content is low, TiO
2The content height is difficult to the powder used in metallurgy reduced iron powder of production high added value, thereby weakens the vitality of this technology.
(3) summary of the invention
The objective of the invention is to utilize carry out microwave radiation heating to contain the sefstromite concentrate pelletizing of compound additive, the control process conditions are produced the natural micro alloy iron powder, also contain the multiple beneficial elements such as vanadium, titanium, chromium, cobalt and nickel of trace in product iron powder purity height, the composition, and be solid solution condition and evenly distribute.
The present invention finishes according to the following steps:
1. sefstromite concentrate accounts for the 60%-90% powder through being broken for granularity less than 75um;
2. join the coke, the 0-5% additive sulfuric acid sodium (Na that account for sefstromite concentrate weight 10-20% in the powder
2SO
4), the 0-5% iron powder, making diameter is the 0.8-1.5cm pelletizing;
3. pelletizing carries out drying, and temperature is that 130-150 ℃, time are 30-40min;
4. dry back pelletizing is in the microwave furnace reduction, in join the 20%-50% that accounts for sefstromite concentrate weight the reducing agent coke, the pelletizing reduction temperature is 1100-1300 ℃, the recovery time is 60-120min;
5. the pelletizing ball milling is sized to the powder of granularity less than 180um;
6. use hydrogen reducing again, hydrogen usage is per kilogram powder 5-7L/min, and reduction temperature 750-850 ℃, recovery time 120-240min make the micro alloy iron powder of granularity less than 180um.The advantage that has compared with prior art:
The advantage of heating using microwave is that selectivity adds thermal material, and heating rate is fast, and efficiency of heating surface height, microwave have certain penetrability, can solve " the problem of cold " center " that traditional heating produces; Reducing agent carbon is a kind of extraordinary microwave absorbing material, can be arrived 1053-1556K by heating using microwave in a short period of time, and the localized hyperthermia of carbon can promote the carrying out of cloth Dorr reaction and improve the concentration of CO; In the carbon thermal reduction process, total reaction rate is the control that is subjected to the gasification reaction of carbon, can shorten the recovery time, and sefstromite concentrate also belongs to strong absorbing material, and microwave can promote the endothermic reaction and exothermic reaction simultaneously, and chemical reaction is had catalytic action; Microwave energy can make atom and molecule generation vibration at high speed, and for chemical reaction creates more strong thermodynamic condition, heating using microwave has the effect that reduces chemical reaction temperature in addition, can reduce lattice diffusion activation energy and promote reaction to carry out.Also contain the multiple beneficial elements such as vanadium, titanium, chromium, cobalt and nickel of trace in this handicraft product iron powder purity height, the composition, and be solid solution condition and evenly distribute.
(4) description of drawings: Fig. 1 is a process chart of the present invention
(5) specific embodiment:
Embodiment one:
Material chemical component: TFe 65.32～68.67%, V
2O
50.55 TiO～0.62%,
211.56 SiO～12.42%,
24.89～5.23, Al
2O
34.81～4.94%, CaO 1.38～1.65%, MgO 3.10～3.75%.
Raw material is broken for granularity accounts for 60% powder, join the coke, the 5% additive sulfuric acid sodium (Na that account for sefstromite concentrate weight 10% in the powder less than 75um
2SO
4), to make diameter be the 0.8-1.1cm pelletizing; Pelletizing carries out drying, and temperature is that 130-140 ℃, time are 30min; Dry back pelletizing is in the microwave furnace reduction, and microwave power 700W, frequency 2450MHz join 30% the reducing agent coke that accounts for sefstromite concentrate weight outward, and the pelletizing reduction temperature is 1100-1150 ℃, and the recovery time is 60min; Afterwards the pelletizing ball milling is sized to the powder of granularity less than 180um; Use hydrogen reducing in Muffle furnace, hydrogen usage is per kilogram powder 5-6L/min, and reduction temperature 820-850 ℃, recovery time 120min make the micro alloy iron powder of granularity less than 180um.The iron powder grade is 92.50%.
Embodiment two:
Material chemical component TFe 64.37～67.56%, V
2O
50.52 TiO～0.59%,
211.76 SiO～12.95%,
24.82～5.19, Al
2O
34.64～4.73%, CaO 1.42～1.59%, MgO 3.34～3.69%.
Raw material is broken for granularity accounts for 80% powder, join the coke, the 5% additive sulfuric acid sodium (Na that account for sefstromite concentrate weight 15% in the powder less than 75um
2SO
4), 3% iron powder; Making diameter is the 0.9-1.2cm pelletizing, and pelletizing carries out drying, and temperature is that 140-150 ℃, time are 35min; Dry back pelletizing is in the microwave furnace reduction, and microwave power 700W, frequency 2450MHz join 40% the reducing agent coke that accounts for sefstromite concentrate weight outward, and the pelletizing reduction temperature is 1200-1250 ℃, and the recovery time is 90min; Afterwards the pelletizing ball milling is sized to the powder of granularity less than 180um; Use hydrogen reducing in Muffle furnace, hydrogen usage is per kilogram powder 6-7L/min, and reduction temperature 750-780 ℃, recovery time 180min make the micro alloy iron powder of granularity less than 180um.The iron powder grade is 93.60%.
Embodiment three:
Material chemical component TFe 66.87～69.17%, V
2O
50.49 TiO～0.58%,
211.95 SiO～12.37%,
24.95～5.21, AL
2O
34.71～5.03%, CaO 1.49～1.60%, MgO 3.42～3.62%;
Raw material is broken for granularity accounts for 90% powder, join the coke, the 3% additive sulfuric acid sodium (Na that account for sefstromite concentrate weight 20% in the powder less than 75um
2SO
4), 5% iron powder; Making diameter is the 1.0-1.3cm pelletizing, and pelletizing carries out drying, and temperature is that 130-150 ℃, time are 40min; Dry back pelletizing is in the microwave furnace reduction, and microwave power 700W, frequency 2450MHz join 40% the reducing agent coke that accounts for sefstromite concentrate weight outward, and the pelletizing reduction temperature is 1200-1300 ℃, and the recovery time is 90min; Afterwards the pelletizing ball milling is sized to the powder of granularity less than 180um; Use hydrogen reducing in Muffle furnace, hydrogen usage is per kilogram powder 6-7L/min, and reduction temperature 780-850 ℃, recovery time 240min make the micro alloy iron powder of granularity less than 180um.The iron powder grade is 96.96%.
Claims (4)
1, a kind of method of preparing natural micro alloy iron powder from vanadium-titanium-iron headings by microwave radiation is characterized in that: invention is finished according to the following steps:
1). sefstromite concentrate accounts for the 60%-90% powder through being broken for granularity less than 75um;
2). join the coke, 0-5% additive sulfuric acid sodium, the 0-5% iron powder that account for sefstromite concentrate weight 10-20% in the powder, making diameter is the 0.8-1.5cm pelletizing;
3). pelletizing carries out drying, and temperature is that 130-150 ℃, time are 30-40min;
4). dry back pelletizing is in the microwave furnace reduction, in join the 20%-50% that accounts for sefstromite concentrate weight the reducing agent coke, the pelletizing reduction temperature is 1100-1300 ℃, the recovery time is 60-120min;
5). the pelletizing ball milling is sized to the powder of granularity less than 180um;
6). use hydrogen reducing again, hydrogen usage is per kilogram powder 5-7L/min, and reduction temperature 750-850 ℃, recovery time 120-240min make the micro alloy iron powder of granularity less than 180um.
2, follow method according to the described preparing natural micro alloy iron powder from vanadium-titanium-iron headings by microwave radiation of claim 1, it is characterized in that: for composition is TFe 65.32～68.67%, V
2O
50.55 TiO～0.62%,
211.56 SiO～12.42%,
24.89～5.23, Al
2O
34.81～4.94%, CaO1.38～1.65%, the sefstromite concentrate of MgO 3.10～3.75%, controlled condition is: raw material is broken for granularity and accounts for 60% powder less than 75um, join 10% coke in the powder, 5% additive sulfuric acid sodium, making diameter is the 0.8-1.1cm pelletizing, 130-140 ℃ of pelletizing baking temperature, time 30min, dry back pelletizing is in the microwave furnace reduction, microwave power 700W, frequency 2450MHz, in join 30% reducing agent coke, 1100-1150 ℃ of pelletizing reduction temperature, recovery time 60min, afterwards pelletizing is ground and be sized to the powder of granularity less than 180um, use hydrogen reducing in Muffle furnace, hydrogen usage is per kilogram powder 5-6L/min, reduction temperature 820-850 ℃, recovery time 120min makes the micro alloy iron powder of granularity less than 180um.
3, follow method according to the described preparing natural micro alloy iron powder from vanadium-titanium-iron headings by microwave radiation of claim 1, it is characterized in that: for composition is TFe 64.37～67.56%, V
2O
50.52 TiO～0.59%,
211.76 SiO～12.95%,
24.82～5.19, Al
2O
34.64～4.73%, CaO 1.42～1.59%, the sefstromite concentrate of MgO 3.34～3.69%, controlled condition is: raw material is broken for granularity and accounts for 80% powder less than 75um, join 15% coke in the powder, 5% additive sulfuric acid sodium, 3% iron powder, making diameter is the 0.9-1.2cm pelletizing, the pelletizing baking temperature is 140-150 ℃, time is 35min, dry back pelletizing is in the microwave furnace reduction, microwave power 700W, frequency 2450MHz, in join 40% reducing agent coke, the pelletizing reduction temperature is 1200-1250 ℃, and the recovery time is 90min, pelletizing is ground to be sized to the powder of granularity less than 180um afterwards, in Muffle furnace, use hydrogen reducing, hydrogen usage is per kilogram powder 6-7L/min, reduction temperature 750-780 ℃, recovery time 180min makes the micro alloy iron powder of granularity less than 180um.
4, follow method according to the described preparing natural micro alloy iron powder from vanadium-titanium-iron headings by microwave radiation of claim 1, it is characterized in that: for composition is TFe 66.87～69.17%, V
2O
50.49 TiO～0.58%,
211.95 SiO～12.37%,
24.95～5.21, Al
2O
34.71～5.03%, CaO 1.49～1.60%, the sefstromite concentrate of MgO 3.42～3.62%, controlled condition is: raw material is broken for granularity and accounts for 90% powder less than 75um, join 20% coke in the powder, 3% additive sulfuric acid sodium, 5% iron powder, making diameter is the 1.0-1.3cm pelletizing, the pelletizing baking temperature is 130-150 ℃, time is 40min, dry back pelletizing is in the microwave furnace reduction, microwave power 700W, frequency 2450MHz, in join 40% reducing agent coke, 1200-1300 ℃ of pelletizing reduction temperature, recovery time 90min grinds pelletizing afterwards and is sized to the powder of granularity less than 180um, in Muffle furnace, use hydrogen reducing, hydrogen usage is per kilogram powder 6-7L/min, reduction temperature 780-850 ℃, recovery time 240min makes the micro alloy iron powder of granularity less than 180um.
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Cited By (10)
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| CN100357457C (en) * | 2006-04-04 | 2007-12-26 | 太原理工大学 | Metal ferrochromium preparing method by computer-controlled double microwave ovens |
| CN102343300A (en) * | 2011-08-17 | 2012-02-08 | 昆明理工大学 | Pretreatment method of magnetite |
| CN102794455A (en) * | 2012-09-05 | 2012-11-28 | 昆明理工大学 | Method for preparing primary reduction iron powder by combining inner and outer carbon matching and microwave heating |
| CN102839250A (en) * | 2012-09-28 | 2012-12-26 | 昆明理工大学 | Method for collecting high-quality coal gas in process of producing reduced iron powder by means of microwave heating |
| CN103643041A (en) * | 2013-12-20 | 2014-03-19 | 长沙市东新矿冶科技开发有限公司 | Novel technology for preparing low vanadium-titanium alloy comminuted steel shot through vanadium and titanium iron concentrate |
| CN105014090A (en) * | 2015-07-08 | 2015-11-04 | 上海大学 | Method for preparing TiFe alloy by reducing ferrotitanium oxide under microwave field |
| CN109351968A (en) * | 2018-09-03 | 2019-02-19 | 江苏钛谷科技有限公司 | A kind of technique using microwave mode processing metal powder |
| CN111872412A (en) * | 2020-07-30 | 2020-11-03 | 钢研晟华科技股份有限公司 | Preparation method of metal iron powder for powder metallurgy |
| CN112159880A (en) * | 2020-09-30 | 2021-01-01 | 华北理工大学 | Method and device for making iron by hydrogen |
| CN113528813A (en) * | 2021-08-04 | 2021-10-22 | 攀枝花金原科技有限公司 | Preparation method of iron powder and vanadium-rich titanium material |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US3202503A (en) * | 1960-07-05 | 1965-08-24 | Yawata Iron & Steel Co | Production of high quality steel from iron sand |
| DE3791011C2 (en) * | 1987-09-17 | 1990-07-19 | Inst Gornogo Dela Sibirskogo O | |
| CN1034264C (en) * | 1991-03-23 | 1997-03-19 | 冶金工业部长沙矿冶研究院 | Method for preparing microalloy iron powder by reduction grinding and selecting method |
| CN1069110C (en) * | 1999-04-30 | 2001-08-01 | 中南工业大学 | Technology for comprehensive utilization of V-Ti magnetite |
| CN1070535C (en) * | 1999-04-30 | 2001-09-05 | 中南工业大学 | Quick reduction process for cold solidified spheroids of iron concentrate in rotary kiln |
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2005
- 2005-04-25 CN CNB2005100107669A patent/CN1319684C/en not_active Expired - Fee Related
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| CN100357457C (en) * | 2006-04-04 | 2007-12-26 | 太原理工大学 | Metal ferrochromium preparing method by computer-controlled double microwave ovens |
| CN102343300A (en) * | 2011-08-17 | 2012-02-08 | 昆明理工大学 | Pretreatment method of magnetite |
| CN102794455B (en) * | 2012-09-05 | 2014-10-01 | 昆明理工大学 | Method for preparing primary reduction iron powder by combining inner and outer carbon matching and microwave heating |
| CN102794455A (en) * | 2012-09-05 | 2012-11-28 | 昆明理工大学 | Method for preparing primary reduction iron powder by combining inner and outer carbon matching and microwave heating |
| CN102839250A (en) * | 2012-09-28 | 2012-12-26 | 昆明理工大学 | Method for collecting high-quality coal gas in process of producing reduced iron powder by means of microwave heating |
| CN102839250B (en) * | 2012-09-28 | 2014-07-30 | 昆明理工大学 | Method for collecting high-quality coal gas in process of producing reduced iron powder by means of microwave heating |
| CN103643041A (en) * | 2013-12-20 | 2014-03-19 | 长沙市东新矿冶科技开发有限公司 | Novel technology for preparing low vanadium-titanium alloy comminuted steel shot through vanadium and titanium iron concentrate |
| CN105014090A (en) * | 2015-07-08 | 2015-11-04 | 上海大学 | Method for preparing TiFe alloy by reducing ferrotitanium oxide under microwave field |
| CN109351968A (en) * | 2018-09-03 | 2019-02-19 | 江苏钛谷科技有限公司 | A kind of technique using microwave mode processing metal powder |
| CN111872412A (en) * | 2020-07-30 | 2020-11-03 | 钢研晟华科技股份有限公司 | Preparation method of metal iron powder for powder metallurgy |
| CN112159880A (en) * | 2020-09-30 | 2021-01-01 | 华北理工大学 | Method and device for making iron by hydrogen |
| CN112159880B (en) * | 2020-09-30 | 2022-03-29 | 华北理工大学 | Method and device for making iron by hydrogen |
| CN113528813A (en) * | 2021-08-04 | 2021-10-22 | 攀枝花金原科技有限公司 | Preparation method of iron powder and vanadium-rich titanium material |
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