CN1382635A - Process for preparing iron oxide black from iron sludge generated in iron powder reduction technology - Google Patents
Process for preparing iron oxide black from iron sludge generated in iron powder reduction technology Download PDFInfo
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- CN1382635A CN1382635A CN 02115960 CN02115960A CN1382635A CN 1382635 A CN1382635 A CN 1382635A CN 02115960 CN02115960 CN 02115960 CN 02115960 A CN02115960 A CN 02115960A CN 1382635 A CN1382635 A CN 1382635A
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- iron
- oxide black
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- iron powder
- mud
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Abstract
A process for preparing iron oxide black from the iron mud generated in reducing iron powder includes synthesizing while adding reducing ageing in ratio of wt.% 1:0.1-0.2, pressure filter, regulating slurry, sieving, water washing, pressure filter and drying.
Description
Technical field
The present invention relates to a kind of production method of iron oxide black, particularly a kind of is the method for raw material production iron oxide black with the iron mud that produces in the iron powder reducing technology.
Background technology
At present, be that the reduction reaction of reductive agent is a kind of traditional reducing process with the iron powder, as: by the multiple arylamine of nitro-compound reduction preparation; With aldehyde, ketone, the acid reduction corresponding alcohol of preparation or hydrocarbon compound; Prepare phenol by quinones; By sulfocompound reduction preparation thiophenol or-sulfinic acid.The iron powder reducing method has characteristics such as technology is simple, low for equipment requirements, side reaction is few, and is applied widely, but low owing to producing a large amount of iron mud grades behind the iron powder reducing, normal discarded, usually causes the wasting of resources, causes environmental pollution.Though traditional iron oxide black production method product performance are good, because preparation consumes material cost height, product price height.
Summary of the invention
Purpose of the present invention is exactly that will to provide a kind of be the method for raw material production iron oxide black with the iron mud that produces in the iron powder reducing technology, adopt the iron oxide black excellent property of this method preparation, and processing cost is cheap.
The object of the present invention is achieved like this: a kind of is the method for raw material production iron oxide black with the iron mud that produces in the iron powder reducing technology, may further comprise the steps:
(a) synthetic: (major ingredient is Fe with iron mud
3O
4And Fe
2O
3) drop in the reactor, after adding water and stirring, add the reductive agent of iron mud weight 10%-20%, under the normal pressure temperature of reaction 90-95 ℃, stirred mixing speed 80-100 rev/min 9 hours;
(b) press filtration: the whole pumps of suspension that (a) building-up reactions is generated obtain solid formation A to the plate-and-frame filter press press filtration;
(c) size mixing: solid formation A is added add water to the surge tank and size mixing, the weight ratio of solid formation A and water is 1: 1, dispersed with stirring under the normal temperature and pressure, and mixing speed is 40-60 rev/min;
(d) sieve: the suspension pump after will sizing mixing to trommel screen sieves, and sieve number is the 320-400 order;
(e) washing: to water washing tank, it is colourless to add the supreme layer of hot wash clear liquid with the screen underflow pump, and the weight ratio of screen underflow and hot water is 1: 5, and the hot water temperature is 60 ℃-90 ℃;
(f) press filtration: will wash suspension pump to the plate-and-frame filter press press filtration, and obtain solid formation B;
(g) drying: solid formation B is carried out drying, the iron oxide black finished product, drying temperature is at 50 ℃-300 ℃, 20-60 minute time of drying.
Wherein the reductive agent described in the step (a) is an iron powder.
Wherein (main component is Fe to the solid formation A described in step (b), (c) for synthetic iron mud
3O
4) and the mixture of the intact reductive agent iron powder of unreacted.
Wherein (main component is Fe to the solid formation B described in step (f), (g) for synthetic iron mud
3O
4).
Provided by the invention is the method for raw material production iron oxide black with the iron mud that produces in the iron powder reducing technology, can with the iron mud that produces in the iron powder reducing technology raw material, realized utilization of waste material, reduced environmental pollution, and the iron oxide black by the present invention's preparation is functional, meets relevant national standard.
Description of drawings
The invention will be further described below in conjunction with drawings and Examples.
Fig. 1 is a process flow sheet of the present invention.
Fig. 1 double as Figure of abstract.
Embodiment
As shown in Figure 1, a kind of is the method for raw material production iron oxide black with the iron mud that produces in the iron powder reducing technology, may further comprise the steps:
(a) synthetic: (major ingredient is Fe with iron mud
3O
4And Fe
2O
3) drop in the reactor, after adding water and stirring, add the reductive agent of iron mud weight 10%-20%, under the normal pressure temperature of reaction 90-95 ℃, stirred mixing speed 80-100 rev/min 9 hours;
(b) press filtration: the whole pumps of suspension that (a) building-up reactions is generated obtain solid formation A to the plate-and-frame filter press press filtration;
(c) size mixing: solid formation A is added add water to the surge tank and size mixing, the weight ratio of solid formation A and water is 1: 1, dispersed with stirring under the normal temperature and pressure, and mixing speed is 40-60 rev/min;
(d) sieve: the suspension pump after will sizing mixing to trommel screen sieves, and sieve number is the 320-450 order;
(e) washing: to water washing tank, it is colourless to add the supreme layer of hot wash clear liquid with the screen underflow pump, and the weight ratio of screen underflow and hot water is 1: 5, and the hot water temperature is 60 ℃-90 ℃;
(f) press filtration: will wash suspension pump to the plate-and-frame filter press press filtration, and obtain solid formation B;
(g) drying: solid formation B is carried out drying, the iron oxide black finished product, drying temperature is at 50 ℃-300 ℃, 20-60 minute time of drying.
Wherein the reductive agent described in the step (a) is an iron powder.
Wherein (main component is Fe to the solid formation A described in step (b), (c) for synthetic iron mud
3O
4) and the mixture of the intact reductive agent iron powder of unreacted.
Wherein (main component is Fe to the solid formation B described in step (f), (g) for synthetic iron mud
3O
4).
Embodiment 1:
Get that (major ingredient is Fe with the iron mud that produces in the iron powder reducing technology
3O
4And Fe
3O
3) 100g (containing moisture 20%), add in 250 ml beakers, add 250 ml water dispersed with stirring, add the iron powder of 10g then in the beaker, carry out building-up reactions, 90 ℃ of temperature of reaction, stir after 9 hours, with the suspension filter paper filtering, (main component is Fe with filter cake
3O
4Mixture with the intact iron powder of unreacted) about 115g throws in 500 ml beakers, adding about 500 ml waters while throwing sizes mixing, under the normal temperature and pressure dispersed with stirring evenly after, cross 325 eye mesh screens, sieve aperture 45um, is colourless with screen underflow with 60 ℃ hot wash to upper strata clear liquid, and then uses filter paper filtering, and (main component is Fe with filter cake
3O
4) insert in the CLS101-1E type loft drier, in 100 ± 5 ℃ of oven dry 20 minutes, promptly get iron oxide black finished product 95g.
Embodiment 2:
Get that (major ingredient is Fe with the iron mud that produces in the iron powder reducing technology
3O
4And Fe
2O
3) 500g (containing moisture 20%), add in 500 ml beakers, add 400 ml water dispersed with stirring, add the iron powder of 75g then in the beaker, carry out building-up reactions, 93 ℃ of temperature of reaction, stir after 9 hours, with the suspension filter paper filtering, (main component is Fe with filter cake
3O
4Mixture with the intact iron powder of unreacted) about 500g throws in 500 ml beakers, adding about 500 ml waters while throwing sizes mixing, under the normal temperature and pressure dispersed with stirring evenly after, cross 325 eye mesh screens, sieve aperture 45um, is colourless with screen underflow with 75 ℃ of hot washes to upper strata clear liquid, and then uses filter paper filtering, and (main component is Fe with filter cake
3O
4) insert in the CLS101-1E type loft drier, in 100 ± 5 ℃ of oven dry 30 minutes, promptly get iron oxide black finished product 490g.
Embodiment 3:
Get that (major ingredient is Fe with the iron mud that produces in the iron powder reducing technology
3O
4And Fe
2O
3) 500Kg (containing moisture 20%), be added in the reactor, add and throw the water-dispersion of the about 600L vapor condensation of limit adding, 85 rev/mins of reactor mixing speed, after being uniformly dispersed, add 100Kg reductive agent iron powder in reactor, guarantee 95 ℃ of temperature of reaction, behind the stirring reaction 9 hours, with the whole pumps of suspension in the reactor to the plate-and-frame filter press press filtration.(main component is Fe with filter cake after the press filtration
3O
4Mixture with the intact iron powder of unreacted) about 500Kg adds to surge tank, adds about 500L tap water while throwing and sizes mixing, and after being uniformly dispersed under the normal temperature and pressure, usefulness is pumped in the trommel screen that the order number is 325 orders (sieve aperture is the 45um metallic sieve) sieves.Screen underflow is pumped in the water washing tank, after adding 90 ℃ hot wash and leaving standstill clarification, bleeds off supernatant liquid, the reheat water washing for several times, until supernatant liquid (the about at every turn 2m of amount of water that becomes colorless
3, washing operates under the normal pressure to be carried out), pump is to the plate-and-frame filter press press filtration then, and (main component is Fe with filter cake
3O
4) send into GS * 800 type Rotatingandflashstreamingdrier dryings, controlled temperature is 110 ℃, 60 minutes time of drying.Promptly get iron oxide black finished product 490Kg.
Claims (4)
1, a kind of is the method for raw material production iron oxide black with the iron mud that produces in the iron powder reducing technology, it is characterized in that: may further comprise the steps:
(a) synthetic: (major ingredient is Fe with iron mud
3O
4And Fe
2O
3) drop in the reactor, after adding water and stirring, add the reductive agent of iron mud weight 10%-20%, under the normal pressure temperature of reaction 90-95 ℃, stirred mixing speed 80-100 rev/min 9 hours;
(b) press filtration: the whole pumps of suspension that (a) building-up reactions is generated obtain solid formation A to the plate-and-frame filter press press filtration;
(c) size mixing: solid formation A is added add water to the surge tank and size mixing, the weight ratio of solid formation A and water is 1: 1, dispersed with stirring under the normal temperature and pressure, and mixing speed is 40-60 rev/min;
(d) sieve: the suspension pump after will sizing mixing to trommel screen sieves, and sieve number is the 320-450 order;
(e) washing: to water washing tank, it is colourless to add the supreme layer of hot wash clear liquid with the screen underflow pump, and the weight ratio of screen underflow and hot water is 1: 5, and the hot water temperature is 60 ℃-90 ℃;
(f) press filtration: will wash suspension pump to the plate-and-frame filter press press filtration, and obtain solid formation B;
(g) drying: solid formation B is carried out drying, the iron oxide black finished product, drying temperature is at 50 ℃-300 ℃, 20-60 minute time of drying.
2, according to claim 1 a kind of be the method for raw material production iron oxide black with the iron mud that produces in the iron powder reducing technology, it is characterized in that: wherein the reductive agent described in the step (a) is an iron powder.
3, according to claim 1 a kind of be the method for raw material production iron oxide black with the iron mud that produces in the iron powder reducing technology, it is characterized in that: wherein (main component is Fe to the solid formation A described in step (b), (c) for synthetic iron mud
3O
4) and the mixture of the intact reductive agent iron powder of unreacted.
4, according to claim 1 a kind of be the method for raw material production iron oxide black with the iron mud that produces in the iron powder reducing technology, it is characterized in that: wherein (main component is Fe to the solid formation B described in step (f), (g) for synthetic iron mud
3O
4).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021159602A CN1160255C (en) | 2002-06-11 | 2002-06-11 | Process for preparing iron oxide black from iron sludge generated in iron powder reduction technology |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021159602A CN1160255C (en) | 2002-06-11 | 2002-06-11 | Process for preparing iron oxide black from iron sludge generated in iron powder reduction technology |
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| Publication Number | Publication Date |
|---|---|
| CN1382635A true CN1382635A (en) | 2002-12-04 |
| CN1160255C CN1160255C (en) | 2004-08-04 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB021159602A Expired - Fee Related CN1160255C (en) | 2002-06-11 | 2002-06-11 | Process for preparing iron oxide black from iron sludge generated in iron powder reduction technology |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100408704C (en) * | 2007-04-13 | 2008-08-06 | 北京科技大学 | Method for producing nano-magnetic FeO particle by iron extracted and utilized in tin tails |
| CN102826614A (en) * | 2012-08-31 | 2012-12-19 | 长春工程学院 | Method for preparing iron oxide black by recovering iron in sludge water from biological iron and manganese removal water plant |
| CN104140127A (en) * | 2013-05-09 | 2014-11-12 | 中国科学院过程工程研究所 | Method for producing ferriferrous oxide by using ferric oxide as raw material |
| CN105154104A (en) * | 2015-09-28 | 2015-12-16 | 江苏振宇环保科技有限公司 | Method for preparing soil powder curing agents through recycled iron slime |
| CN109574088A (en) * | 2018-11-26 | 2019-04-05 | 天津市国润永泰环保科技有限公司 | The method and its application of iron black removal product removal of impurities are produced using waste |
| CN114602353A (en) * | 2022-04-13 | 2022-06-10 | 铜陵瑞莱科技有限公司 | Washing device for obtaining low-viscosity iron oxide yellow |
-
2002
- 2002-06-11 CN CNB021159602A patent/CN1160255C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100408704C (en) * | 2007-04-13 | 2008-08-06 | 北京科技大学 | Method for producing nano-magnetic FeO particle by iron extracted and utilized in tin tails |
| CN102826614A (en) * | 2012-08-31 | 2012-12-19 | 长春工程学院 | Method for preparing iron oxide black by recovering iron in sludge water from biological iron and manganese removal water plant |
| CN102826614B (en) * | 2012-08-31 | 2014-03-05 | 长春工程学院 | Method for preparing iron oxide black by recovering iron in sludge water from biological iron and manganese removal water plant |
| CN104140127A (en) * | 2013-05-09 | 2014-11-12 | 中国科学院过程工程研究所 | Method for producing ferriferrous oxide by using ferric oxide as raw material |
| CN104140127B (en) * | 2013-05-09 | 2015-09-30 | 中国科学院过程工程研究所 | A kind of take ferric oxide as the method for raw material production Z 250 |
| CN105154104A (en) * | 2015-09-28 | 2015-12-16 | 江苏振宇环保科技有限公司 | Method for preparing soil powder curing agents through recycled iron slime |
| CN109574088A (en) * | 2018-11-26 | 2019-04-05 | 天津市国润永泰环保科技有限公司 | The method and its application of iron black removal product removal of impurities are produced using waste |
| CN114602353A (en) * | 2022-04-13 | 2022-06-10 | 铜陵瑞莱科技有限公司 | Washing device for obtaining low-viscosity iron oxide yellow |
| CN114602353B (en) * | 2022-04-13 | 2024-04-05 | 铜陵瑞莱科技有限公司 | Washing device for obtaining low-viscosity iron oxide yellow |
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| Publication number | Publication date |
|---|---|
| CN1160255C (en) | 2004-08-04 |
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