CN1559715A - Recovery method of nanometer iron powder from cold rolling emulsion liquid - Google Patents
Recovery method of nanometer iron powder from cold rolling emulsion liquid Download PDFInfo
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- CN1559715A CN1559715A CNA200410012152XA CN200410012152A CN1559715A CN 1559715 A CN1559715 A CN 1559715A CN A200410012152X A CNA200410012152X A CN A200410012152XA CN 200410012152 A CN200410012152 A CN 200410012152A CN 1559715 A CN1559715 A CN 1559715A
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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
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Abstract
A method for recovering the iron nanoparticles from the emulsion used by cold rolling includes such steps as centrifugal separation to remove the most of dirt oil, and washing with detergent which is prepared from Na2CO3, Na2SiO3, detergent TX-10, n-butanol and water through proportional mixing.
Description
Technical field
The present invention relates to a kind of method that from cold-rolling emulsion magnetic filtration product, reclaims nanometer iron powder.
Technical background
Along with China's automobile and household electrical appliances industrial expansion, to the demand of cold-rolled steel sheet also in continuous increase.Need emulsion constantly is sprayed between roll and the steel plate in cold rolling production process, cold-rolling emulsion is mixed through mechanical stirring by water and ROLLING OIL, plays cooling, cleans and lubricates.Costing an arm and a leg of ROLLING OIL is one of main consumable material of cold rolling mill, and therefore, emulsion recycles in cold rolling production.Because thereby the huge fricative a large amount of iron powders between roll and the steel plate make the emulsion downgrade influence quality of cold-rolled products in the cold-rolled process, and the content increase of iron powder can make the emulsion life cycle shorten in the emulsion, the increase production cost.So filtration unit all has been installed in the emulsion of cold rolling mill, what adopted before the nineties in last century is filter paper or filter cloth filtration unit, can filter (micron) iron particle bigger in the emulsion, in order to filter (nanometer) iron particle less in the emulsion, each cold rolling mill has increased magnetic filter again after the nineties.
The magnetic filtration product of general medium-sized cold rolling mill every day is about 400Kg, and the magnetic filtration product contains the ROLLING OIL of the iron powder and 80% (weight percent) of have an appointment 20% (weight percent).Be to bury or burn to the treatment process of magnetic filtration product in the past, not only wasted resource but also contaminate environment.
The preparation method of nanometer iron powder is in the experimental study stage mostly at present, and preparation method commonly used has sputtering method, hybrid plasma method, the precipitator method, hydrolysis method, spray method, laser synthesis method etc.The granularity that the nanometer iron powder that these methods are produced has is inhomogeneous, and the cost height.
Present method is extracted nanometer iron powder based on resource reutilization from industrial waste-cold-rolling emulsion magnetic filtration product, raw material is easy to get, and is with low cost, and the iron particle size that obtains distributes comparatively concentrated.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of nanometer iron powder method that reclaims with low cost from the magnetic filtration product of cold-rolling emulsion.
The present invention adopts following technical scheme:
1. pretreating raw material carries out centrifugation with the high speed settling centrifuge to raw material, to the cold-rolling emulsion pre-treatment, to remove most of greasy dirt.Raw material after the separation divides two-layer up and down, and the upper strata is an oil, and lower floor is the oil-containing iron powder, removes the oil on upper strata.
2. clean pretreated oil-containing iron powder
At first prepare clean-out system, clean-out system adopts following ratio of weight and number component:
Na
2CO
3 1-10
Na
2SiO
3 1-5
Detergent TX-10 0.3-2
Propyl carbinol 0.3-2
Water 90-100
By prescription each component is mixed.
The detailed cleaning process of first iron powder is as follows:
The 1st washing: the clean-out system adding is equipped with in the container of oil-containing iron powder material, both ratios of weight and number are 4: 1 to 6: 1, be heated to 70-80 ℃ and keep this temperature, behind the mechanical stirring 100-130min, centrifugation on whizzer, be divided into three layers after the separation from top to bottom promptly: oil, clean-out system and iron powder, carry out rinsing with isolated iron powder with clean water.
Isolated iron powder can directly carry out the 2nd washing without the clean water rinsing: the iron powder that will wash centrifugal back lower floor for the first time carries out 2 washings with new clean-out system.Repeat cleaning process the 1st time, only the wash agitation time is become 35-40min, be divided into three layers after the centrifugation from top to bottom promptly: oil, clean-out system and iron powder.Skim uppermost oil reservoir, the intermediary clean-out system uses when staying the 1st cleaning doing next cleaning process.Carry out the isolated iron powder in the washing back second time and can directly carry out the clean water rinsing, also can directly carry out following washing for the third time.
Isolated iron powder carries out the 3rd washing: the iron powder of the 2nd the centrifugal back of washing lower floor is carried out 3 washings with new clean-out system.Repeat cleaning process the 1st time, only the wash agitation time is become 35-40min, be divided into three layers after the separation from top to bottom promptly: oil, clean-out system and iron powder.Skim uppermost oil reservoir, the intermediary clean-out system uses when staying the 2nd cleaning doing next cleaning process.Isolated iron powder carries out rinsing with clean water again.
3. rinsing: the iron powder after first, second or the washing for the third time can be carried out rinsing respectively, also can carry out continuously earlier carrying out rinsing at last after three washings, promptly after the washing, with clean water rinsing 4 times.The rinsing temperature is at 70-80 ℃, mechanical stirring, and each churning time is 10-15min, centrifugation then.During the 1st rinsing the rinsing liquid after the centrifugation is outwelled, stayed the 1st rinsing doing next cleaning process to use the rinsing liquid after the centrifugation during the 2nd rinsing.Stay the 2nd rinsing doing next cleaning process to use the rinsing liquid after the centrifugation during the 3rd rinsing.Stay the 3rd rinsing doing next cleaning process to use the rinsing liquid after the centrifugation during the 4th rinsing.
When the second batch of iron powder cleaned, clean-out system and the rinsing liquid that stays with first cleaning process in order during the quantity not sufficient of clean-out system and rinsing liquid, suitably added new polishing.When washing for the third time with new clean-out system, during the 4th rinsing with new clean water.Other is identical with first cleaning process.
Later cleaning and the like.
4. at the loft drier inner drying, drying temperature is 50-60 ℃ to drying, finally obtains the nanometer iron powder of clean dried with the iron powder of wash clean.
Positively effect of the present invention is as follows: the clean-out system of employing autogamy of the present invention washs the oil-containing iron powder with lower floor after the centrifugal separation method pre-treatment, thoroughly to remove the greasy dirt on iron powder surface, mechanical stirring during each cleaning process washing of the present invention, gradient washing.Each cleaning process is divided once washing, a rinsing, and for reaching washing effect preferably, each cleaning process also can be divided three continuous washing, last rinsing.Present method is extracted nanometer iron powder based on resource reutilization from industrial waste-cold-rolling emulsion magnetic filtration product, raw material is easy to get, and is with low cost, and the iron particle size that obtains distributes comparatively concentrated.
Description of drawings
The iron powder sem photograph of accompanying drawing for adopting technology of the present invention to reclaim
Embodiment
Embodiment 1
Stand-by by following formulated clean-out system 500ml:
Na
2CO
3 8
Na
2SiO
3 3
Detergent TX-10 2
Propyl carbinol 0.3
Water 100
Get magnetic filtration product 100g from rolling mill production line, with the centrifugation on whizzer of magnetic filtration product.The rotating speed of whizzer is 10000 rev/mins, and centrifugation time is 35min, and most of ROLLING OIL of separating in the magnetic filtration product of back floats over the upper strata, and lower floor is the oil-containing iron powder, claims to such an extent that the weight of oil-containing iron powder is 22g.
The 1st washing poured the clean-out system for preparing in the container that the oil-containing iron powder is housed into, both weight ratios are 6: 1, are heated to 75 ℃ and keep this temperature, behind the mechanical stirring 125min, centrifugation 15min on whizzer is divided into three layers promptly from top to bottom after the separation: oil, clean-out system and iron powder.Outwell upper two layers.
The iron powder that the 2nd washing will be washed centrifugal back lower floor for the first time carries out 2 washings with new clean-out system.Repeat cleaning process the 1st time, only washing time is become 35min, be divided into three layers after the centrifugation from top to bottom promptly: oil, clean-out system and iron powder.Skim uppermost oil reservoir, the intermediary clean-out system uses when staying the 1st cleaning doing next cleaning process.
The 3rd washing carried out 3 washings with the iron powder of the 2nd the centrifugal back of washing lower floor with new clean-out system.Repeat cleaning process the 1st time, only washing time is become 35min, be divided into three layers after the centrifugation from top to bottom promptly: oil, clean-out system and iron powder.Skim uppermost oil reservoir, the intermediary clean-out system uses when staying the 2nd cleaning doing next cleaning process.
Use pure water rinsing 4 times after the rinsing washing.Each water consumption 100ml, the rinsing temperature is at 75 ℃, mechanical stirring 10min, centrifugation 15min then.During the 1st rinsing the rinsing liquid after the centrifugation is outwelled, stayed the 1st rinsing doing next cleaning process to use the rinsing liquid after the centrifugation during the 2nd rinsing.Stay the 2nd rinsing doing next cleaning process to use the rinsing liquid after the centrifugation during the 3rd rinsing.Stay the 3rd rinsing doing next cleaning process to use the rinsing liquid after the centrifugation during the 4th rinsing.
(4) dry iron powder vacuum-drying in loft drier with wash clean, drying temperature is 50 ℃, obtains iron powder 14.3 grams of clean dry.
After testing, the clean rate of iron powder is 96.5%, and the scanning electron microscope picture of iron powder is seen accompanying drawing, and therefrom the granularity that can find out iron powder is nanometer iron powder below 100nm.
Embodiment 2
Stand-by by following formulated clean-out system 500ml:
Na
2CO
3 10
Na
2SiO
3 1
Detergent TX-10 1
Propyl carbinol 2
Water 95
Get magnetic filtration product 110g from rolling mill production line, with the centrifugation on whizzer of magnetic filtration product.The rotating speed of whizzer is 10000 rev/mins, and centrifugation time is 35min, and most of ROLLING OIL of separating in the magnetic filtration product of back floats over the upper strata, and lower floor is the oil-containing iron powder, claims to such an extent that the weight of oil-containing iron powder is 24g.
The 1st washing poured the clean-out system for preparing in the container that the oil-containing iron powder is housed into, both weight ratios are 5: 1, are heated to 70 ℃ and keep this temperature, behind the mechanical stirring 100min, centrifugation 15min on whizzer is divided into three layers promptly from top to bottom after the separation: oil, clean-out system and iron powder.Outwell upper two layers.
The iron powder that the 2nd washing will be washed centrifugal back lower floor for the first time carries out 2 washings with new clean-out system.Repeat cleaning process the 1st time, only washing time is become 37min, be divided into three layers after the centrifugation from top to bottom promptly: oil, clean-out system and iron powder.Skim uppermost oil reservoir, the intermediary clean-out system uses when staying the 1st cleaning doing next cleaning process.
The 3rd washing carried out 3 washings with the iron powder of the 2nd the centrifugal back of washing lower floor with new clean-out system.Repeat cleaning process the 1st time, only washing time is become 37min, be divided into three layers after the centrifugation from top to bottom promptly: oil, clean-out system and iron powder.Skim uppermost oil reservoir, the intermediary clean-out system uses when staying the 2nd cleaning doing next cleaning process.
Use pure water rinsing 4 times after the rinsing washing.Each water consumption 100ml, the rinsing temperature is at 70 ℃, mechanical stirring 12min, centrifugation 15min then.During the 1st rinsing the rinsing liquid after the centrifugation is outwelled, stayed the 1st rinsing doing next cleaning process to use the rinsing liquid after the centrifugation during the 2nd rinsing.Stay the 2nd rinsing doing next cleaning process to use the rinsing liquid after the centrifugation during the 3rd rinsing.Stay the 3rd rinsing doing next cleaning process to use the rinsing liquid after the centrifugation during the 4th rinsing.
(4) dry iron powder vacuum-drying in loft drier with wash clean, drying temperature is 55 ℃, obtains iron powder 15.6 grams of clean dry.
After testing, the clean rate of iron powder is 96.1%, and the scanning electron microscope picture of iron powder is seen accompanying drawing, and therefrom the granularity that can find out iron powder is nanometer iron powder below 100nm.
Embodiment 3
Stand-by by following formulated clean-out system 500ml:
Na
2CO
3 3
Na
2SiO
3 5
Detergent TX-10 0.3
Propyl carbinol 1
Water 90
Get magnetic filtration product 120g from rolling mill production line, with the centrifugation on whizzer of magnetic filtration product.The rotating speed of whizzer is 10000 rev/mins, and centrifugation time is 35min, and most of ROLLING OIL of separating in the magnetic filtration product of back floats over the upper strata, and lower floor is the oil-containing iron powder, claims to such an extent that the weight of oil-containing iron powder is 26g.
The 1st washing poured the clean-out system for preparing in the container that the oil-containing iron powder is housed into, both weight ratios are 4: 1, are heated to 80 ℃ and keep this temperature, behind the mechanical stirring 130min, centrifugation 15min on whizzer is divided into three layers promptly from top to bottom after the separation: oil, clean-out system and iron powder.Outwell upper two layers.
The iron powder that the 2nd washing will be washed centrifugal back lower floor for the first time carries out 2 washings with new clean-out system.Repeat cleaning process the 1st time, only washing time is become 40min, be divided into three layers after the centrifugation from top to bottom promptly: oil, clean-out system and iron powder.Skim uppermost oil reservoir, the intermediary clean-out system uses when staying the 1st cleaning doing next cleaning process.
The 3rd washing carried out 3 washings with the iron powder of the 2nd the centrifugal back of washing lower floor with new clean-out system.Repeat cleaning process the 1st time, only washing time is become 40min, be divided into three layers after the centrifugation from top to bottom promptly: oil, clean-out system and iron powder.Skim uppermost oil reservoir, the intermediary clean-out system uses when staying the 2nd cleaning doing next cleaning process.
Want rinsing 4 times after the rinsing washing, the rinsing temperature is at 70,75 or 80 ℃, mechanical stirring 10,12 or 15min, centrifugation 15min then.Use the rinsing liquid that centrifugation obtains after the cleaning process rinsing for the second time during rinsing for the first time, add the suitable quantity of water polishing during rinsing liquid deficiency 100ml.Use the rinsing liquid that centrifugation obtains after the cleaning process rinsing for the third time during rinsing for the second time, add the suitable quantity of water polishing during rinsing liquid is not enough 100ml.Use the rinsing liquid that centrifugation obtains after the 4th rinsing of a cleaning process during rinsing for the third time, rinsing liquid adds the suitable quantity of water polishing when not enough.Use 100ml water during the 4th rinsing.During rinsing for the first time, the rinsing liquid after the centrifugation is outwelled, second and third, during four rinsings, the rinsing liquid after the centrifugation is stayed first, second and third time use of doing next cleaning process respectively.
(4) dry iron powder vacuum-drying in loft drier with wash clean, drying temperature is 60 ℃, obtains iron powder 16.5 grams of clean dry.
After testing, the clean rate of iron powder is 96.2%, and the scanning electron microscope picture of iron powder is seen accompanying drawing, and therefrom the granularity that can find out iron powder is nanometer iron powder below 100nm.
Claims (6)
1, the recovery method of nanometer iron powder in a kind of cold-rolling emulsion, the method that it is characterized in that using centrifugation is removed most of greasy dirt to the cold-rolling emulsion pre-treatment; Wash pretreated oil-containing iron powder material with clean-out system, described clean-out system is made up of following ratio of weight and number component:
Na
2CO
3 1-10
Na
2SiO
3 1-5
Detergent TX-10 0.3-2
Propyl carbinol 0.3-2
Water 90-100
By prescription each component is mixed.
Clean-out system is added in the container that the oil-containing iron powder material after the processing is housed, and both ratios of weight and number are 4: 1 to 6: 1, are heated to 70-80 ℃ and keep this temperature, behind the mechanical stirring 100-130min, centrifugation on whizzer, isolated iron powder carries out rinsing with clean water again.
2, the recovery method of nanometer iron powder in a kind of cold-rolling emulsion according to claim 1 is characterized in that the above-mentioned iron powder that centrifugation goes out after washing is for the first time washed once more with new clean-out system.Repeat above-mentioned cleaning process, only the wash agitation time is become 35-40min, the iron powder that centrifugation goes out carries out rinsing with clean water again.
3, the recovery method of nanometer iron powder in a kind of cold-rolling emulsion according to claim 2 is characterized in that the above-mentioned iron powder that centrifugation goes out after washing is for the second time carried out the 3rd washing.Repeat cleaning process the 1st time, only the wash agitation time is become 35-40min, the centrifugal iron powder of telling carries out rinsing with clean water again.
4,, it is characterized in that described rinsing promptly uses the clean water rinsing 4 times according to the recovery method of nanometer iron powder in claim 1, the 2 or 3 described a kind of cold-rolling emulsions.The rinsing temperature is at 70-80 ℃, mechanical stirring, and each churning time is 10-15min, centrifugation then.During the 1st rinsing the rinsing liquid after the centrifugation is outwelled, stayed the 1st rinsing doing next cleaning process to use the rinsing liquid after the centrifugation during the 2nd rinsing.Stay the 2nd rinsing doing next cleaning process to use the rinsing liquid after the centrifugation during the 3rd rinsing.Stay the 3rd rinsing doing next cleaning process to use the rinsing liquid after the centrifugation during the 4th rinsing.
5, according to the recovery method of nanometer iron powder in claim 1, the 2 or 3 described a kind of cold-rolling emulsions, it is characterized in that iron powder with wash clean at the loft drier inner drying, drying temperature is 50-60 ℃, finally obtains the nanometer iron powder of clean dried.
6, the recovery method of nanometer iron powder in a kind of cold-rolling emulsion according to claim 4 is characterized in that iron powder with wash clean at the loft drier inner drying, and drying temperature is 50-60 ℃, finally obtains the nanometer iron powder of clean dried.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200410012152XA CN1260335C (en) | 2004-02-20 | 2004-02-20 | Recovery method of nanometer iron powder from cold rolling emulsion liquid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200410012152XA CN1260335C (en) | 2004-02-20 | 2004-02-20 | Recovery method of nanometer iron powder from cold rolling emulsion liquid |
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|---|---|
| CN1559715A true CN1559715A (en) | 2005-01-05 |
| CN1260335C CN1260335C (en) | 2006-06-21 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB200410012152XA Expired - Fee Related CN1260335C (en) | 2004-02-20 | 2004-02-20 | Recovery method of nanometer iron powder from cold rolling emulsion liquid |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100446900C (en) * | 2006-08-17 | 2008-12-31 | 王惠民 | Cutting production technology of metal nanometer powder zero boundry particle |
| CN102489053A (en) * | 2011-12-20 | 2012-06-13 | 华东理工大学 | Method and device for removing fine solid particles in cold continuous rolling emulsified liquid |
| CN102581270A (en) * | 2012-03-21 | 2012-07-18 | 石家庄市宏晟环保科技有限公司 | Method for recycling iron powder in magnetic filters of cold rolling factory |
| CN102632231A (en) * | 2012-03-21 | 2012-08-15 | 河北科技大学 | Cleaning agent for recycling iron powder from magnetic filtered product in cold rolling plant |
| CN104946893A (en) * | 2015-06-09 | 2015-09-30 | 武汉钢铁(集团)公司 | Method of extracting superfine iron from cold rolling greasy filth |
| CN107903941A (en) * | 2017-11-27 | 2018-04-13 | 黄河三角洲京博化工研究院有限公司 | A kind of separation and recovery method of waste mineral oil |
| CN111715709A (en) * | 2020-06-16 | 2020-09-29 | 江门绿润环保科技有限公司 | Method for recovering nano iron powder |
| CN112892856A (en) * | 2021-01-14 | 2021-06-04 | 武汉乾冶众联科技有限公司 | Cold rolling waste treatment method |
-
2004
- 2004-02-20 CN CNB200410012152XA patent/CN1260335C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100446900C (en) * | 2006-08-17 | 2008-12-31 | 王惠民 | Cutting production technology of metal nanometer powder zero boundry particle |
| CN102489053A (en) * | 2011-12-20 | 2012-06-13 | 华东理工大学 | Method and device for removing fine solid particles in cold continuous rolling emulsified liquid |
| CN102581270A (en) * | 2012-03-21 | 2012-07-18 | 石家庄市宏晟环保科技有限公司 | Method for recycling iron powder in magnetic filters of cold rolling factory |
| CN102632231A (en) * | 2012-03-21 | 2012-08-15 | 河北科技大学 | Cleaning agent for recycling iron powder from magnetic filtered product in cold rolling plant |
| CN104946893A (en) * | 2015-06-09 | 2015-09-30 | 武汉钢铁(集团)公司 | Method of extracting superfine iron from cold rolling greasy filth |
| CN104946893B (en) * | 2015-06-09 | 2017-05-17 | 武汉钢铁(集团)公司 | Method of extracting superfine iron from cold rolling greasy filth |
| CN107903941A (en) * | 2017-11-27 | 2018-04-13 | 黄河三角洲京博化工研究院有限公司 | A kind of separation and recovery method of waste mineral oil |
| CN111715709A (en) * | 2020-06-16 | 2020-09-29 | 江门绿润环保科技有限公司 | Method for recovering nano iron powder |
| CN112892856A (en) * | 2021-01-14 | 2021-06-04 | 武汉乾冶众联科技有限公司 | Cold rolling waste treatment method |
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| Publication number | Publication date |
|---|---|
| CN1260335C (en) | 2006-06-21 |
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Assignee: Shijiazhuang Hongsheng Environmental Protection Technology Co., Ltd. Assignor: Hebei University of Science and Technology Contract record no.: 2011130000143 Denomination of invention: Recovery method of nanometer iron powder from cold rolling emulsion liquid Granted publication date: 20060621 License type: Exclusive License Open date: 20050105 Record date: 20110921 |
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