CN107082428A - A kind of method that cementite is prepared using many metal sulfate slags - Google Patents
A kind of method that cementite is prepared using many metal sulfate slags Download PDFInfo
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- CN107082428A CN107082428A CN201710296260.1A CN201710296260A CN107082428A CN 107082428 A CN107082428 A CN 107082428A CN 201710296260 A CN201710296260 A CN 201710296260A CN 107082428 A CN107082428 A CN 107082428A
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Abstract
The present invention discloses a kind of method that cementite is prepared using many metal sulfate slags, including：Many metal sulfate slags are well mixed with binding agent, chlorinating agent, and pelletizing material is made；The pelletizing material is made into green-ball and chlorination is heated after drying, then in CO+CO2+H2Or CH4+H2Carry out cooling down in carburizing, inert atmosphere in gas, obtain pelletizing after carburizing；Pelletizing after the carburizing is carried out carrying out wet magnetic separation after wet ball-milling, ball milling, cementite is dried to obtain.The method that the present invention is provided prepares cementite efficient quick, with low cost, energy-conserving and environment-protective.
Description
Technical field
The present invention relates to a kind of field of metallurgy, more particularly to a kind of method that cementite is prepared using many metal sulfate slags.
Background technology
As a kind of important secondary resource, sulfate slag contains a small amount of copper, lead, zinc not only containing abundant iron
Deng non-ferrous metal.The Iron grade of sulfate slag is generally 30%~63%, is significantly higher than the iron ore average grade of China 33%, it contains
The non-ferrous metals such as some copper, lead, zinc also have considerable recovery value.According to statistics, the sulphur of China's about 15,000,000 tons of discharge every year
Acid sludge, the sulfate slag stored up more is up to more than one hundred million tons, and this part of sulfuric acid slag not only pollutes environment, occupied cultivated land, and it contains
Non-ferrous metal also bring harm to human body.As the accessory substance after pyrite-based sulfuric acid production, the Iron grade of sulfate slag is relatively low,
The non-ferrous metal content such as copper, lead, zinc is higher, the embedding cloth relation and complicated occurrence state of mineral.These features cause current sulfuric acid
Choosing, the smelting of slag are difficult, and the added value utilized is not high.
The utilization of many metal sulfate slags mainly includes following method both at home and abroad at present：
Traditional gravity treatment, flotation and magnetic separation process processing sulfate slag, be by sulfate slag be milled down to after certain particle size further according to
The difference of the density of iron mineral and gangue, magnetic and surface nature, can be respectively adopted gravity treatment, magnetic separation and flotation to separate and reclaim
Iron mineral, then iron ore concentrate can be prepared by filtering and drying.
Sulfate slag is added directly into sinter mixture or pellet feed, then by sintering process or pelletizing process system
It is standby go out sintering deposit or pellet.
Chlorinating roasting handles sulfate slag, is that chlorinating agent is added in sulfate slag, then carries out middle temperature at 800-1000 DEG C
Non-ferrous metal is removed by wet-leaching roasted ore after chloridising roasting, then iron ore concentrate is obtained by magnetic separation；Or in 1000-1200
Volatilizable removing after high temperature chlorination roasting, non-ferrous metal generation chloride is carried out between DEG C, the pelletizing after roasting is again in 1200-
High-temperature roasting is carried out between 1350 DEG C and prepares oxide pellet for blast furnace process.
Chloridising roasting-direct-reduction-magnetic method processing sulfate slag, is to prepare balling-up after adding chlorinating agent in sulfate slag
Group, then carries out high temperature chlorination roasting removing non-ferrous metal between 1000-1200 DEG C, after obtained agglomerates addition bituminous coal
It is reduced directly, obtained direct-reduction pelletizing is purified metals iron by ball milling and magnetic separation process, is finally obtained high-grade
Reduced iron powder.
Existing technology mainly has the disadvantage that：Traditional gravity treatment, flotation and magnetic separation process preparation process can not remove copper,
The non-ferrous metals such as lead, zinc, the iron ore concentrate added value of preparation is low, also needs just prepare blast furnace burden by multistep pyroprocess.
The non-ferrous metal content such as copper, lead, zinc in sintering deposit or pellet, the sintering deposit or pellet of preparation is prepared with sulfate slag
Height, copper can influence the quality of steel, and lead, zinc can cause furnace nodulation, and because the Iron grade of sulfate slag is not high, this can be reduced
The Iron grade of sintering deposit or pellet, so as to cause the increase of blast furnace ironmaking process energy consumption.Chloridizing roast in medium tempera-ture handles sulfate slag,
The iron ore concentrate of preparation also needs to just prepare blast furnace burden by multistep pyroprocess, and wet method leaching process treating capacity is big；
And high temperature chlorination roasting process can only handle the high sulfate slag of Iron grade.Chloridising roasting-direct-reduction-magnetic method processing sulfuric acid
Slag, easily the reduced iron powder activity height of preparation, oxidation, particularly mechanical milling process are easier to aoxidize.Due to active high, reduced iron powder
Spontaneous combustion is also easy in storage and transportation.
The content of the invention
In view of this, the present invention provides a kind of method that cementite can be prepared using many metal sulfate slags, can either take off
Non-ferrous metal in sulphur removal acid sludge, can prepare cementite, be effectively utilized sulfate slag again.
To solve above technical problem, the technical scheme is that utilizing the preparation carbonization of many metal sulfate slags using a kind of
The method of iron, including：
Many metal sulfate slags are well mixed with binding agent, chlorinating agent, and pelletizing material is made；
Described pelletizing material is made into green-ball and chlorination is heated after drying, then in CO+CO2+H2Or CH4+H2Oozed in gas
Cooled down in carbon, inert atmosphere, obtain pelletizing after carburizing；
Pelletizing after the carburizing is carried out carrying out wet magnetic separation after wet ball-milling, ball milling, cementite is dried to obtain.
It is preferred that, pelletizing material is made and specifically includes：
Added water when many metal sulfate slags are mixed with binding agent, chlorinating agent, be well mixed, obtain pelletizing material.
It is preferred that, described chlorinating agent is in calcium chloride, sodium chloride, potassium chloride, magnesium chloride, ferric trichloride and ammonium chloride
One or more.
It is preferred that, the consumption of chlorinating agent described by weight percentage is 0-10%.
It is preferred that, described binding agent is bentonite or calcium hydroxide.
It is preferred that, described consumption of binder scope is 0-3%.
It is preferred that, heating chlorination by the dry bulb specifically, be heated to 1000- after the pelletizing material is made green-ball and dried
Between 1200 DEG C, the chlorination of 0-40 minutes is carried out；
The temperature of the pelletizing carburizing is 550-800 DEG C, carburizing time is 30-300min.
It is preferred that, the gas CO+CO that the carburizing is used2+H2Middle CO：CO2：H2Volume ratio is (50~100)：(0~
30)：(0~20)；
Or the CH4+H2Middle CH4：H2Volume ratio is (10~100)：(0~90).
It is preferred that, described to carry out wet ball-milling by pelletizing after the carburizing, wet magnetic separation is carried out after ball milling is specially：
Pelletizing after carburizing is crushed to granularity less than wet ball-milling is carried out after 1mm, and wet type magnetic is then carried out in magnetic separator
Choosing；
The magnetic field intensity of told magnetic separation process is 50~200mT.
The invention provides a kind of method that cementite is prepared using many metal sulfate slags, wherein the present invention is roasted by chlorination
Burning-carburizing-magnetic method, you can the non-ferrous metal such as removing copper, lead, zinc, can prepare cementite, then pass through ball milling and magnetic separation again
Cheng Tichun cementite, in chlorination process, non-ferrous metal is converted into chloride, and the chloride is in 1000-1200 DEG C of roasting process
In be converted into gas so as to removing of volatilizing, also small part during ball milling and magnetic separation, cementite and gangue separation
Simultaneously separated so that obtain and stable chemical performance higher than the added value of iron ore concentrate and reduced iron powder, it is not oxidizable,
The High Quality Charge Used for EAF cementite of power consumption can be reduced, the high value added utilization of many metal sulfate slags is realized.
Compared with traditional beneficiation method, agglomerates of sintered pellets method and chlorinating roasting processing sulfate slag technique, flow of the present invention
Short, small investment, can directly prepare charging stock for electric furnace, and centre eliminates the process that blast furnace process prepares molten iron.
Embodiment
In order that those skilled in the art more fully understands technical scheme, with reference to embodiment
The present invention is described in further detail.
The invention provides a kind of method that cementite is prepared using many metal sulfate slags, including：
Many metal sulfate slags are well mixed with binding agent, chlorinating agent, and pelletizing material is made；
The pelletizing material is made into green-ball and chlorination is heated after drying, then in CO+CO2+H2Or CH4+H2Oozed in gas
Cooled down in carbon, inert atmosphere, obtain pelletizing after carburizing；
Pelletizing after the carburizing is carried out carrying out wet magnetic separation after wet ball-milling, ball milling, cementite is dried to obtain.
In order to the iron in sulfate slag is separated with other non-ferrous metals, it is necessary to pelletizing operate, first prepare pelletizing material,
Pelletizing material is made to specifically include：
Added water when many metal sulfate slags are mixed with binding agent, chlorinating agent, be well mixed, obtain pelletizing material.It is described
The amount of being preferably added to of water is that the easy balling-up of suitable balling process pelletizing material is all right, it is not necessary to which too many, the binding agent is preferably swollen
Profit soil or calcium hydroxide, most preferably bentonite；Described consumption of binder accounts for the ratio preferably 0-3% of sulfate slag gross weight,
More preferably 1%~3%, most preferably 1.5%~2.5%.
The one kind of described chlorinating agent in calcium chloride, sodium chloride, potassium chloride, magnesium chloride, ferric trichloride and ammonium chloride
Or a variety of, more preferably sodium chloride and calcium chloride.According to the present invention, the consumption of chlorinating agent described by weight percentage accounts for total sulfur
The 0-10% of acid sludge weight, more preferably 2%~9%, most preferably 6%~8%.The effect of chlorinating agent is primarily to make chlorine
Reacted between agent and metal, non-ferrous metal is formed into chloride, and chloride can be changed into gaseous state in high-temperature roasting
Volatilization, so that separating most non-ferrous metal.
After pelletizing material is prepared, green-ball is prepared with pelletizing material, the pelletizing material is made into green-ball and heating chlorine is carried out after drying
Change operation, the heating chlorination specifically, the dry bulb is heated between 1000-1200 DEG C, carry out the chlorination of 0-40 minutes,
More elect 10~30 minutes, most preferably 20~30 minutes as.
After chlorination, remaining iron is subjected to carburizing generation cementite, the temperature of the carburizing is 550-800 DEG C, carburizing when
Between be 30-300min.The gas CO+CO that the carburizing is used2+H2Middle CO：CO2：H2Volume ratio is preferably (50~100)：(0~
30)：(0~20), more preferably (55~80):(10~20)：(5~20), be most preferably (65~75)：(15~20):(10~
20)；
Or the CH4+H2Middle CH4：H2Volume ratio is (10~100)：(0~90), more preferably (30~60)：(20~
70), it is most preferably (40~60)：(40~60).
Described to carry out wet ball-milling by pelletizing after the carburizing after the completion of carburizing, wet magnetic separation is carried out after ball milling is specially：
Pelletizing after carburizing is crushed to granularity less than wet ball-milling is carried out after 1mm, and wet magnetic separation is then carried out in magnetic separator；Told magnetic
The magnetic field intensity for selecting process is 50~200mT.
This law is bright there is provided a kind of method that cementite is prepared using many metal sulfate slags, wherein the present invention is roasted by chlorination
Burning-carburizing-magnetic method, you can the non-ferrous metal such as removing copper, lead, zinc, can prepare cementite, then pass through ball milling and magnetic separation again
Cheng Tichun cementite, in chlorination process, non-ferrous metal is converted into chloride, and the chloride is in 1000-1200 DEG C of roasting process
In be converted into gas so as to removing of volatilizing, also small part during ball milling and magnetic separation, cementite and gangue separation
Simultaneously separated so that obtain and stable chemical performance higher than the added value of iron ore concentrate and reduced iron powder, it is not oxidizable,
The High Quality Charge Used for EAF cementite of power consumption can be reduced, the high value added utilization of many metal sulfate slags is realized.
Compared with traditional beneficiation method, agglomerates of sintered pellets method and chlorinating roasting processing sulfate slag technique, flow of the present invention
Short, small investment, can directly prepare charging stock for electric furnace, and centre eliminates the process that blast furnace process prepares molten iron.
It is specific embodiment below：
Embodiment 1：The Iron grade 59.20% of sulfate slag, copper, lead, the content of zinc are respectively 0.89%, 1.11% and
0.29%, the content that sulfate slag is less than 0.075mm is 78.58%.8%CaCl will be with the addition of2With 1.8% bentonitic sulfate slag
A diameter of 8-16mm green-ball is prepared into after the profit mill 4min in damp mill, profit mill moisture 15%, profit mill in disc balling machine.
Shatter strength of green pellet be 3.9 times/0.5m, green-ball dry after at a temperature of 1100 chlorination 25min.Obtained chlorination pelletizing is 650
DEG C and CO：CO2：H2For 65：15：Carburizing 180min in 20 mixed gas, hot-bulb is cooled down in nitrogen.Pelletizing is crushed after cooling
To less than 1mm.Under conditions of pulp density is 50%, ball milling obtains ball milling fineness 99% less than 200 in conical ball mill
Mesh, then ore pulp magnetic separation in magnetic field intensity is 130mT magnetic separator, can obtain the iron content that is carbonized in concentrate is 88.1%, iron
The rate of recovery 82% cementite.The removal efficiency of copper, lead and zinc is respectively to 90.73%, 98.68% and 87.74%.
Embodiment 2：The Iron grade 56.20% of sulfate slag, copper, lead, the content of zinc are respectively 0.39%, 0.89% and
0.59%, the content that sulfate slag is less than 0.075mm is 86.58%.The bentonitic sulfate slags of 8%NaCl and 1.5% will be with the addition of
A diameter of 8-16mm green-ball is prepared into after the profit mill 3min in damp mill, profit mill moisture 15%, profit mill in disc balling machine.
Shatter strength of green pellet be 3.2 times/0.5m, green-ball dry after at a temperature of 1100 chlorination 30min.Obtained chlorination pelletizing is 650
DEG C and CO：CO2：H2For 70：10：Carburizing 160min in 20 mixed gas, hot-bulb is cooled down in nitrogen.Pelletizing is crushed after cooling
To less than 1mm.Under conditions of pulp density is 50%, ball milling obtains ball milling fineness 100% less than 200 in conical ball mill
Mesh, then ore pulp magnetic separation in magnetic field intensity is 120mT magnetic separator, can obtain concentrate carbonization iron content is 87.3%, iron
The cementite of the rate of recovery 80%.The removal efficiency of copper, lead and zinc is respectively to 89.73%, 97.36% and 85.74%.
Embodiment 3：The Iron grade 49.70% of sulfate slag, copper, lead, the content of zinc are respectively 0.28%, 1.35% and
0.69%, the content that sulfate slag is less than 0.075mm is 80.12%.8%CaCl will be with the addition of2With 2.1% bentonitic sulfate slag
A diameter of 8-16mm green-ball is prepared into after the profit mill 3min in damp mill, profit mill moisture 13%, profit mill in disc balling machine.
Shatter strength of green pellet be 3.5 times/0.5m, green-ball dry after at a temperature of 1100 chlorination 30min.Obtained chlorination pelletizing is 750
DEG C and CH4：H2For 40：Carburizing 80min in 60 mixed gas, hot-bulb is cooled down in nitrogen.Pelletizing, which is crushed to, after cooling is less than
1mm.It is that under conditions of 50%, ball milling obtains ball milling fineness 100% less than 200 mesh in conical ball mill, so in pulp density
Ore pulp magnetic separation in magnetic field intensity is 130mT magnetic separator afterwards, can obtain concentrate carbonization iron content is 85.6%, the rate of recovery of iron
75% cementite.The removal efficiency of copper, lead and zinc is respectively to 91.73%, 98.16% and 86.23%.
Embodiment 4：The Iron grade 38.61% of sulfate slag, copper, lead, the content of zinc are respectively 0.38%, 0.55% and
0.39%, the content that sulfate slag is less than 0.075mm is 80.12%.6%CaCl will be with the addition of2With 2.5% bentonitic sulfate slag
A diameter of 8-16mm green-ball is prepared into after the profit mill 2min in damp mill, profit mill moisture 11%, profit mill in disc balling machine.
Shatter strength of green pellet be 3.3 times/0.5m, green-ball dry after at a temperature of 1075 DEG C chlorination 20min.Obtained chlorination pelletizing exists
650 DEG C and CO：CO2：H2For 65：15：Carburizing 180min in 20 mixed gas, hot-bulb is cooled down in nitrogen.Pelletizing is broken after cooling
Broken arrive is less than 1mm.It is that under conditions of 50%, ball milling obtains ball milling fineness 100% and is less than in conical ball mill in pulp density
200 mesh, then ore pulp magnetic separation in magnetic field intensity is 110mT magnetic separator, can obtain concentrate carbonization iron content is 83.6%, iron
The rate of recovery 72% cementite.The removal efficiency of copper, lead and zinc is respectively to 93.73%, 99.52% and 89.89%.
It the above is only the preferred embodiment of the present invention, it is noted that above-mentioned preferred embodiment is not construed as pair
The limitation of the present invention, protection scope of the present invention should be defined by claim limited range.For the art
For those of ordinary skill, without departing from the spirit and scope of the present invention, some improvements and modifications can also be made, these change
Enter and retouch and also should be regarded as protection scope of the present invention.
Claims (9)
1. a kind of method that cementite is prepared using many metal sulfate slags, it is characterised in that including：
Many metal sulfate slags are well mixed with binding agent, chlorinating agent, and pelletizing material is made；
The pelletizing material is made into green-ball and is calcined after drying, carburizing pelletizing is obtained；
The carburizing is heated after chlorination in CO+CO with pelletizing2+H2Or CH4+H2Carry out cooling down in carburizing, inert atmosphere in gas,
Obtain pelletizing after carburizing；
Pelletizing after the carburizing is carried out carrying out wet magnetic separation after wet ball-milling, ball milling, cementite is dried to obtain.
2. according to the method described in claim 1, it is characterised in that pelletizing material is made and specifically includes：
Added water when many metal sulfate slags are mixed with binding agent, chlorinating agent, be well mixed, obtain pelletizing material.
3. method according to claim 1 or 2, it is characterised in that described chlorinating agent is selected from calcium chloride, sodium chloride, chlorine
Change the one or more in potassium, magnesium chloride, ferric trichloride and ammonium chloride.
4. method according to claim 3, it is characterised in that the consumption of chlorinating agent described by weight percentage is 0-
10%.
5. method according to claim 1 or 2, it is characterised in that described binding agent is bentonite or calcium hydroxide.
6. method according to claim 5, it is characterised in that described consumption of binder scope is 0-3%.
7. according to the method described in claim 1, it is characterised in that chlorination is carried out after the pelletizing material pelletizing is dried specific
For：Dry bulb carries out the chlorination of 0-40 minutes between 1000-1200 DEG C；
The temperature of the pelletizing carburizing is 550-800 DEG C, carburizing time is 30-300min.
8. method according to claim 7, it is characterised in that CO in the gas CO+CO2+H2 that the carburizing is used：CO2：
H2 volume ratios are (50~100)：(0~30)：(0~20)；
Or CH4 in the CH4+H2：H2 volume ratios are (10~100)：(0~90).
9. according to the method described in claim 1, it is characterised in that described that pelletizing after the carburizing is subjected to wet ball-milling, ball
Wet magnetic separation is carried out after mill is specially：
Pelletizing after carburizing is crushed to granularity less than wet ball-milling is carried out after 1mm, and wet magnetic separation is then carried out in magnetic separator；
The magnetic field intensity of told magnetic separation process is 50~200mT.
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| CN108622899A (en) * | 2018-05-31 | 2018-10-09 | 武汉理工大学 | A kind of pure Fe3C raw powder's production technologies |
| CN108677022A (en) * | 2018-06-19 | 2018-10-19 | 苏州大学 | A kind of method that sintering dust separation ash prepares removing harmful element during cementite |
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| CN1807237A (en) * | 2005-12-31 | 2006-07-26 | 武汉科技大学 | Method for preparing iron carbide using iron ore concentrate powder |
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| CN107974559A (en) * | 2017-11-20 | 2018-05-01 | 中国科学院过程工程研究所 | A kind of method that high-quality iron smelting pellets are prepared using pyrite cinder |
| CN108622899A (en) * | 2018-05-31 | 2018-10-09 | 武汉理工大学 | A kind of pure Fe3C raw powder's production technologies |
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