CN104946893B - Method of extracting superfine iron from cold rolling greasy filth - Google Patents
Method of extracting superfine iron from cold rolling greasy filth Download PDFInfo
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- CN104946893B CN104946893B CN201510313748.1A CN201510313748A CN104946893B CN 104946893 B CN104946893 B CN 104946893B CN 201510313748 A CN201510313748 A CN 201510313748A CN 104946893 B CN104946893 B CN 104946893B
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- cold rolling
- greasy filth
- rolling greasy
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- filtering residue
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a method of extracting superfine iron from cold rolling greasy filth. The method is characterized by comprising the following steps: (1) the cold rolling greasy filth is immersed into an ammonium chloride solution with 5-20% of weight percent concentration for mixing, grease is subjected to full quaternization and is filtered, and filter residues are standby; (2) the obtained filter residues are placed into a hexadecyl trimethyl ammonium bromide solution with 5-20% of weight percent concentration for mixing, the grease is fully displaced and is filtered, and filter residues are standby; (3) the obtained filter residues are placed into acetone for mixing, little residual emulsified oil in the filter residues is fully extracted and is filtered, and filter residues are standby; and (4) the obtained filter residues are dried under the temperature of 45-55 DEG C so as to obtain superfine iron. According to the invention, the recovery rate of scrap iron in the cold rolling greasy filth is almost 100%; the amount of hazardous waste is reduced, so that the hazardous waste processing cost of an enterprise is reduced; and high value-added superfine iron products with high purity and high activity can be also obtained.
Description
Technical field
The present invention relates to solid waste resource recovery utilizes technology, ultra-fine ferrum is extracted from cold rolling greasy filth in particular to one kind
Method.
Background technology
In cold-rolling process, in order to the steel billet for rolling is cooled down and lubricated, needs spray emulsifying in the operation of rolling
Liquid, and billet surface is through constantly impact and rolls, the ultra-fine ferrum of surface of steel plate can be flowed in cold-rolling emulsion because of peeling, from
And cold-rolling emulsion is polluted.Cold rolling breast in cold-rolling emulsion purification process, after magnetic bar filter is to pollution
Change liquid to be filtered, adsorb the mixture that the atrament on magnetic bar filter is oil-containing oils and fatss and ultra-fine ferrum, it is this mixed
Compound is commonly referred to as cold rolling greasy filth.At present cold rolling greasy filth is to carry out solidification landfill disposal as danger wastes, but Jing is examined
Analysis is surveyed, substantial amounts of ultra-fine ferrum, such as micron ferrum and Nanoscale Iron are contained in cold rolling greasy filth, ultra-fine ferrum is a kind of very high thing of activity
Matter, is widely used in catalyst and special manufacturing.Therefore, if the ultra-fine ferrum in cold rolling greasy filth can be carried out point with oils and fatss
From, the content of dangerous solid waste on the one hand can be reduced, reduce enterprise's danger wastes disposal and take, on the other hand also can produce
The ultra-fine ferrum of product of raw high added value.
At present, with regard to how to extract ultra-fine ferrum from cold rolling greasy filth, there are reports, and it is mainly by the side of alkali cleaning
Formula is washed to cold rolling greasy filth, to isolate ultra-fine ferrum.This alkali washing method approximately as：Main component is adopted for Na2CO3
And Na2SiO3Alkaline solution as detergent, pretreated cold rolling greasy filth is washed.There is following lacking in said method
Point：
Pretreated oil-containing iron powder material is washed with abluent, abluent is mainly by Na2CO3And Na2SiO3It is molten Deng alkalescence
Liquid is constituted.This kind of method is suffered from the drawback that：1) wash incomplete, the oil emulsion containing a large amount of complicated components in cold rolling greasy filth,
It includes the ROLLING OIL of vegetable oil, mineral oil and other compositions, and there are some researches show, alkali cleaning is higher to vegetable oil clearance, but
It is bad to mineral oil clean result, it is difficult to obtain the ultra-fine ferrum of cleaning；2) detergent alkalescence is relatively strong, to what is contained in cold rolling greasy filth
There is calcination destruction in Nanoscale Iron or micron ferrum, affect the activity of ultra-fine ferrum.
The content of the invention
Present invention aim to provide a kind of method that ultra-fine ferrum is extracted from cold rolling greasy filth, the method can remove cold
The oils and fatss in greasy filth are rolled, the ultra-fine ferrum in cold rolling greasy filth is isolated, the recycling of cold rolling greasy filth is realized.
For achieving the above object, the technical solution used in the present invention is：A kind of side that ultra-fine ferrum is extracted from cold rolling greasy filth
Method, comprises the following steps：
1) cold rolling greasy filth is soaked in the ammonium chloride solution that weight percent concentration is 5~20% and is stirred mixing,
Fully by the Vegetable oil lipoprotein in cold rolling greasy filth and mineral grease ammonium, filtered after then standing a period of time, filtering residue is standby；
2) by step 1) to be placed in the cetyl trimethylammonium bromide that weight percent concentration is 5~20% molten for gained filtering residue
Stirring mixing, fully cements out the Vegetable oil lipoprotein and mineral grease in filtering residue in liquid, carries out after then standing a period of time
Filter, filtering residue is standby；
3) by step 2) gained filtering residue is placed in acetone and mixed, and a small amount of oil emulsion to remaining in filtering residue is carried out
Fully extracting, is filtered after then standing a period of time, and filtering residue is standby；
4) by step 4) gained filtering residue dried at 45~55 DEG C, obtain final product ultra-fine ferrum.
Further, the component and its weight percentage of the cold rolling greasy filth are as follows：20~30% mineral grease, 10
~20% Vegetable oil lipoprotein, 10~20% water, 40~57% ferrum, 3~5% surfactant.
Further, the step 1) in, the consumption of ammonium chloride solution is the cold rolling greasy filth of 10~30ml/g.
Further, the step 2) in, the consumption of cetyl trimethylammonium bromide solution is 5~15ml/g cold-rolled lubricating oils
Mud.
Further, the step 1) in, mixing time is 30~50min, and time of repose is 2~3h.
Further, the step 2) in, mixing time is 30~40min, and time of repose is 2~3h.
Further, the step 3) in, mixing time is 30~50min, and time of repose is 2~3h.
Compared with prior art, the present invention has advantages below：
First, the response rate nearly 100% of the inventive method to iron filings in cold rolling greasy filth, and the iron powder for extracting is particle diameter
In micron order and nano level superfine iron powder, the amount of danger wastes is not only reduced, reduce the danger wastes of enterprise
Cost of disposal, has also obtained the high-purity superfine ferrum product with high added value.
Second, the destruction that alkaline detergent exists to ultra-fine ferrum in cold rolling greasy filth is compared, inventive process avoids
Ultra-fine ferrum is conducive to protecting the activity of Nanoscale Iron and micron ferrum in cold rolling greasy filth by calcination.
Third, the inventive method is good to the removal effect of oils and fatss, the plant in cold rolling greasy filth not only can be well removed
Oils and fatss, also greatly improve the removal effect to mineral grease；Meanwhile, the inventive method causes the emulsifying in ferrum and cold rolling greasy filth
Oil is completely separated and comes, and is conducive to the later-stage utilization of oil emulsion, is conducive to fully realizing the recycling of cold rolling greasy filth.
Description of the drawings
Fig. 1 is the pictorial diagram of the ultra-fine ferrum that embodiment 1 is extracted.
Fig. 2 is the microscopic appearance figure of the ultra-fine ferrum that embodiment 1 is extracted.
Specific embodiment
With reference to specific embodiment, the present invention is described in further detail, is easy to more clearly understand the present invention,
But they do not constitute to the present invention and limit.
Embodiment 1
The component and its weight percentage of cold rolling greasy filth is as follows：27% mineral grease, 10% Vegetable oil lipoprotein, 20%
Water, 40% ferrum, 3% surfactant.
1) take the cold rolling greasy filth of 50g to be placed in the ammonium chloride solution that 1L weight percent concentration is 5%, start agitator to mixed
Close liquid to be stirred, agitator speed is 60~70 turns/min, stirs 45min, fully by the Vegetable oil lipoprotein in cold rolling greasy filth and
Mineral grease ammonium, then the mixed liquor after ammonium is stood filtered after 2.5h, and filtering residue is standby；
2) by step 1) gained filtering residue be placed in the cetyl trimethylammonium bromide that 500ml weight percent concentration is 15%
In solution, start agitator and mixed liquor is stirred, agitator speed is 60~70 turns/min, stir 30min, fully will filter
Most of Vegetable oil lipoprotein and mineral grease in slag is cemented out, and is then stood mixed liquor and filtered after 2.5h, and filtering residue is standby
With；
3) by step 2) gained filtering residue be placed in the acetone of 500ml, start agitator and mixed liquor be stirred, agitator
Rotating speed is 60 turns/min, stirs 45min, and a small amount of oil emulsion to remaining in filtering residue is fully extracted, then that mixed liquor is quiet
Put and filtered after 2h, filtering residue is standby；
4) step 3) gained filtering residue is put in the baking oven with inert gas shielding, at a temperature of 50 DEG C dry, drying
Thing is ultra-fine ferrum.
The ultra-fine ferrum of gained is the clean ultra-fine ferrum of high-purity, and the superfine iron powder particle diameter fine uniform, its pattern in kind is shown in Fig. 1,
Microscopic appearance is shown in Fig. 2；The response rate of ferrum is up to 98% in cold rolling greasy filth.
Embodiment 2
The component and its weight percentage of cold rolling greasy filth is as follows：30% mineral grease, 10% Vegetable oil lipoprotein, 15%
Water, 40% ferrum, 5% surfactant.
1) take the cold rolling greasy filth of 50g to be placed in the ammonium chloride solution that 1L weight percent concentration is 20%, start agitator pair
Mixed liquor is stirred, and agitator speed is 60~70 turns/min, 45min is stirred, fully by the Vegetable oil lipoprotein in cold rolling greasy filth
With mineral grease ammonium, then the mixed liquor after ammonium is stood and filtered after 2.5h, filtering residue is standby；
2) by step 1) gained filtering residue be placed in the cetyl trimethylammonium bromide that 500ml weight percent concentration is 20%
In solution, start agitator and mixed liquor is stirred, agitator speed is 70 turns/min, 40min is stirred, fully by filtering residue
Most of Vegetable oil lipoprotein and mineral grease cement out, then will mixed liquor stand 2.5h after filtered, filtering residue is standby；
3) by step 2) gained filtering residue be placed in the acetone of 500ml, start agitator and mixed liquor be stirred, agitator
Rotating speed is 60~70 turns/min, stirs 45min, and a small amount of oil emulsion to remaining in filtering residue is fully extracted, then will mixing
Liquid stands and filtered after 3h, and filtering residue is standby；
4) step 3) gained filtering residue is put in the baking oven with inert gas shielding, at a temperature of 50 DEG C dry, drying
Thing is ultra-fine ferrum.
The ultra-fine ferrum of gained is the clean ultra-fine ferrum of high-purity；The response rate of ferrum is up to 97% in cold rolling greasy filth.
Embodiment 3
The component and its weight percentage of cold rolling greasy filth is as follows：20% mineral grease, 10% Vegetable oil lipoprotein, 10%
Water, 57% ferrum, 3% surfactant.
1) take the cold rolling greasy filth of 50g to be placed in the ammonium chloride solution that 1L weight percent concentration is 10%, start agitator pair
Mixed liquor is stirred, and agitator speed is 60~70 turns/min, 30min is stirred, fully by the Vegetable oil lipoprotein in cold rolling greasy filth
With mineral grease ammonium, then the mixed liquor after ammonium is stood and filtered after 2h, filtering residue is standby；
2) by step 1) gained filtering residue be placed in the cetyl trimethylammonium bromide that 500ml weight percent concentration is 5%
In solution, start agitator and mixed liquor is stirred, agitator speed is 70 turns/min, 40min is stirred, fully by filtering residue
Most of Vegetable oil lipoprotein and mineral grease cement out, then will mixed liquor stand 3h after filtered, filtering residue is standby；
3) by step 2) gained filtering residue be placed in the acetone of 500ml, start agitator and mixed liquor be stirred, agitator
Rotating speed is 60~70 turns/min, stirs 50min, and a small amount of oil emulsion to remaining in filtering residue is fully extracted, then will mixing
Liquid stands and filtered after 2.5h, and filtering residue is standby；
4) step 3) gained filtering residue is put in the baking oven with inert gas shielding, at a temperature of 55 DEG C dry, drying
Thing is ultra-fine ferrum.
The ultra-fine ferrum of gained is the clean ultra-fine ferrum of high-purity；The response rate of ferrum is up to 100% in cold rolling greasy filth.
Embodiment 4
The component and its weight percentage of cold rolling greasy filth is as follows：25% mineral grease, 15% Vegetable oil lipoprotein, 10%
Water, 46% ferrum, 4% surfactant.
1) take the cold rolling greasy filth of 50g to be placed in the ammonium chloride solution that 1L weight percent concentration is 15%, start agitator pair
Mixed liquor is stirred, and agitator speed is 60~70 turns/min, 50min is stirred, fully by the Vegetable oil lipoprotein in cold rolling greasy filth
With mineral grease ammonium, then the mixed liquor after ammonium is stood and filtered after 3h, filtering residue is standby；
2) by step 1) gained filtering residue be placed in the cetyl trimethylammonium bromide that 500ml weight percent concentration is 15%
In solution, start agitator and mixed liquor is stirred, agitator speed is 70 turns/min, 35min is stirred, fully by filtering residue
Most of Vegetable oil lipoprotein and mineral grease cement out, then will mixed liquor stand 2h after filtered, filtering residue is standby；
3) by step 2) gained filtering residue be placed in the acetone of 500ml, start agitator and mixed liquor be stirred, agitator
Rotating speed is 60~70 turns/min, stirs 30min, and a small amount of oil emulsion to remaining in filtering residue is fully extracted, then will mixing
Liquid stands and filtered after 3h, and filtering residue is standby；
4) step 3) gained filtering residue is put in the baking oven with inert gas shielding, at a temperature of 45 DEG C dry, drying
Thing is ultra-fine ferrum.
The ultra-fine ferrum of gained is the clean ultra-fine ferrum of high-purity；The response rate of ferrum is up to 99% in cold rolling greasy filth.
Claims (7)
1. a kind of method that ultra-fine ferrum is extracted from cold rolling greasy filth, it is characterised in that：Comprise the following steps：
1) cold rolling greasy filth is soaked in the ammonium chloride solution that weight percent concentration is 5~20% and is stirred mixing, fully
By the Vegetable oil lipoprotein in cold rolling greasy filth and mineral grease ammonium, filtered after then standing a period of time, filtering residue is standby；
2) by step 1) gained filtering residue be placed in the cetyl trimethylammonium bromide solution that weight percent concentration is 5~20%
Stirring mixing, fully cements out the Vegetable oil lipoprotein and mineral grease in filtering residue, is filtered after then standing a period of time,
Filtering residue is standby；
3) by step 2) gained filtering residue is placed in acetone and mixed, and a small amount of oil emulsion to remaining in filtering residue is carried out fully
Extracting, is filtered after then standing a period of time, and filtering residue is standby；
4) by step 3) gained filtering residue dried at 45~55 DEG C, obtain final product ultra-fine ferrum.
2. the method for extracting ultra-fine ferrum from cold rolling greasy filth according to claim 1, it is characterised in that：The cold rolling greasy filth
Component and its weight percentage are as follows：20~30% mineral grease, 10~20% Vegetable oil lipoprotein, 10~20% water,
40~57% ferrum, 3~5% surfactant.
3. the method that ultra-fine ferrum is extracted from cold rolling greasy filth according to claim 1 or claim 2, it is characterised in that：The step 1)
In, the consumption of ammonium chloride solution is the cold rolling greasy filth of 10~30ml/g.
4. the method that ultra-fine ferrum is extracted from cold rolling greasy filth according to claim 1 or claim 2, it is characterised in that：The step 2)
In, the consumption of cetyl trimethylammonium bromide solution is the cold rolling greasy filth of 5~15ml/g.
5. the method that ultra-fine ferrum is extracted from cold rolling greasy filth according to claim 1 or claim 2, it is characterised in that：The step 1)
In, mixing time is 30~50min, and time of repose is 2~3h.
6. the method that ultra-fine ferrum is extracted from cold rolling greasy filth according to claim 1 or claim 2, it is characterised in that：The step 2)
In, mixing time is 30~40min, and time of repose is 2~3h.
7. the method that ultra-fine ferrum is extracted from cold rolling greasy filth according to claim 1 or claim 2, it is characterised in that：The step 3)
In, mixing time is 30~50min, and time of repose is 2~3h.
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| CN201510313748.1A CN104946893B (en) | 2015-06-09 | 2015-06-09 | Method of extracting superfine iron from cold rolling greasy filth |
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| CN201510313748.1A CN104946893B (en) | 2015-06-09 | 2015-06-09 | Method of extracting superfine iron from cold rolling greasy filth |
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| CN104946893B true CN104946893B (en) | 2017-05-17 |
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| CN110723874A (en) * | 2019-09-20 | 2020-01-24 | 宁波宝新不锈钢有限公司 | Solid-liquid separation method of rolling oil sludge |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1559715A (en) * | 2004-02-20 | 2005-01-05 | 河北科技大学 | Recovery method of nanometer iron powder from cold rolling emulsion liquid |
| CN1560324A (en) * | 2004-02-20 | 2005-01-05 | 河北科技大学 | Oil strain cleaning agent for ferrous metal powder |
| CN104004581A (en) * | 2013-02-22 | 2014-08-27 | 宝山钢铁股份有限公司 | Rolled oil sludge purifying method |
| CN104498717A (en) * | 2014-12-02 | 2015-04-08 | 上海应用技术学院 | Recovery method for metal powder in rolling oil sludge |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7632332B2 (en) * | 2006-12-12 | 2009-12-15 | Honda Motor Co., Ltd. | Preparation of iron-titanium nanoparticles |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1559715A (en) * | 2004-02-20 | 2005-01-05 | 河北科技大学 | Recovery method of nanometer iron powder from cold rolling emulsion liquid |
| CN1560324A (en) * | 2004-02-20 | 2005-01-05 | 河北科技大学 | Oil strain cleaning agent for ferrous metal powder |
| CN104004581A (en) * | 2013-02-22 | 2014-08-27 | 宝山钢铁股份有限公司 | Rolled oil sludge purifying method |
| CN104498717A (en) * | 2014-12-02 | 2015-04-08 | 上海应用技术学院 | Recovery method for metal powder in rolling oil sludge |
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Effective date of registration: 20170731 Address after: 430083, Hubei Wuhan Qingshan District Factory No. 2 Gate joint stock company organs Patentee after: Wuhan iron and Steel Company Limited Address before: 15 Wuchang, Wuhan Friendship Avenue, No. 999, block A, layer (Wuhan Iron and steel science and technology innovation department), No. 430080, Patentee before: Wuhan Iron & Steel (Group) Corp. |
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