CN1160255C - 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 PDF

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Publication number
CN1160255C
CN1160255C CNB021159602A CN02115960A CN1160255C CN 1160255 C CN1160255 C CN 1160255C CN B021159602 A CNB021159602 A CN B021159602A CN 02115960 A CN02115960 A CN 02115960A CN 1160255 C CN1160255 C CN 1160255C
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China
Prior art keywords
iron
solid formation
oxide black
mud
iron powder
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CN1382635A (en
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时克勤
韩军
胡修权
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ZHIJIANG KAIYUAN CHEMICAL CO Ltd
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ZHIJIANG KAIYUAN CHEMICAL CO Ltd
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Abstract

The present invention discloses a method for preparing iron oxide black by using iron mud generated in an iron powder reduction technology as a raw material, which comprises the processes of synthesis, pressing filtration, pulp regulation, sieving, water washing, pressing filtration and drying, wherein a proper quantity of reducing agent is added to the synthesis process, and the weight ratio of the iron mud to the reducing agent is from 1:0.1 to 0.2. The present invention can realize the comprehensive utilization of iron mud waste slag.

Description

With the iron mud that produces in the iron powder reducing technology is the method for raw material production iron oxide black
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, the reduction reaction take iron powder as reducing agent is a kind of traditional reducing process, 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; Prepare thiophenol or sulfinic acid by reduction of sulfur-contained compound.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.Although traditional iron oxide black production method properties of product are good, because preparation consumes cost of raw material 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 is synthetic: be Fe with Main Ingredients and Appearance 3O 4And Fe 2O 3Iron mud drop in the reactor, after adding water and stirring, add the iron powder of iron mud weight 10%-20%, under the normal pressure reaction temperature 90-95 ℃, stirred speed of agitator 80-100 rev/min 9 hours;
The 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 sizes 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 sieves: the suspension pump after will sizing mixing to rotary screen sieves, and sieve number is the 320-400 order;
The 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;
The 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 solid formation A described in step b, the c is that main component is Fe 3O 4Synthetic iron mud and the mixture of the complete reducing agent iron powder of unreacted.
Wherein the solid formation B described in step f, the g is that main component is Fe 3O 4Synthetic iron mud.
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 is synthetic: be Fe with Main Ingredients and Appearance 3O 4And Fe 2O 3Iron mud drop in the reactor, after adding water and stirring, add the iron powder of iron mud weight 10%-20%, under the normal pressure reaction temperature 90-95 ℃, stirred speed of agitator 80-100 rev/min 9 hours;
The 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 sizes 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 sieves: the suspension pump after will sizing mixing to rotary screen sieves, and sieve number is the 320-450 order;
The 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;
The 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 solid formation A described in step b, the c is that main component is Fe 3O 4Synthetic iron mud and the mixture of the complete reducing agent iron powder of unreacted.
Wherein the solid formation B described in step f, the g is that main component is Fe 3O 4Synthetic iron mud.
Embodiment 1:
Get the Main Ingredients and Appearance that produces in the iron powder reducing technology as Fe 3O 4And Fe 2O 3And the iron mud 100g of moisture content 20% adds in 250 ml beakers, adds 250 ml water dispersed with stirring, add then the iron powder of 10g in the beaker, carry out synthetic reaction, 90 ℃ of reaction temperatures, stirring after 9 hours, with the suspension Filter paper filtering, is Fe with main component 3O 4Filter cake with the mixture of the complete 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 screenings with 60 ℃ hot wash to upper strata clear liquid, and then use Filter paper filtering, be Fe with main component 3O 4Filter cake insert in the CLS101-1E type drying box, in 100 ± 5 ℃ the oven dry 20 minutes, namely get iron oxide black finished product 95g.
Embodiment 2:
Get the Main Ingredients and Appearance that produces in the iron powder reducing technology as Fe 3O 4And Fe 2O 3And the iron mud 500g of moisture content 20% adds in 500 ml beakers, adds 400 ml water dispersed with stirring, add then the iron powder of 75g in the beaker, carry out synthetic reaction, 93 ℃ of reaction temperatures, stirring after 9 hours, with the suspension Filter paper filtering, is Fe with main component 3O 4Filter cake and the filter cake of the mixture of the complete 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 screenings with 75 ℃ of hot washes to upper strata clear liquid, and then use Filter paper filtering, be Fe with main component 3O 4Filter cake insert in the CLS101-1E type drying box, in 100 ± 5 ℃ the oven dry 30 minutes, namely get iron oxide black finished product 490g.
Embodiment 3:
Get the Main Ingredients and Appearance that produces in the iron powder reducing technology as Fe 3O 4And Fe 2O 3And the iron mud 500Kg of moisture content 20%, be added in the reactor, add and throw the aqueous dispersion of the about 600L steam-condensation of limit adding, 85 rev/mins of reactor speeds of agitator, after being uniformly dispersed, add 100Kg reducing agent iron powder in reactor, guarantee 95 ℃ of reaction temperatures, behind the stirring reaction 9 hours, with the whole pumps of suspension in the reactor to the plate and frame filter press press filtration.After the press filtration, be Fe with main component 3O 4With the filter cake of the mixture of the complete iron powder of unreacted, about 500Kg adds to surge tank, adds about 500L running water while throwing and sizes mixing, and after being uniformly dispersed under the normal temperature and pressure, sieves with being pumped in the rotary screen that the order number is 325 orders (sieve aperture is the 45um metallic sieve).Screenings is pumped in the water washing tank, after adding 90 ℃ hot wash and leaving standstill clarification, bleeds off supernatant liquor, again the heating water washing for several times, (amount of water is about 2m at every turn until supernatant liquor becomes colorless 3, washing operates under the normal pressure to be carried out), pump is Fe to the plate and frame filter press press filtration with main component then 3O 4Filter cake send into GS * 800 type Rotatingandflashstreamingdrier dryings, control temperature be 110 ℃, 60 minutes drying times.Namely get iron oxide black finished product 490Kg.

Claims (3)

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 is synthetic: be Fe with Main Ingredients and Appearance 3O 4And Fe 2O 3Iron mud drop in the reactor, after adding water and stirring, add the iron powder of iron mud weight 10%-20%, under the normal pressure reaction temperature 90-95 ℃, stirred speed of agitator 80-100 rev/min 9 hours;
The 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 sizes 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 sieves: the suspension pump after will sizing mixing to rotary screen sieves, and sieve number is the 320-450 order;
The 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;
The 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, a kind of iron mud that produces in the iron powder reducing technology according to claim 1 method of producing iron oxide black as raw material, it is characterized in that: wherein the solid formation A described in step b, the c is that main component is Fe 3O 4Synthetic iron mud and the mixture of the complete reducing agent iron powder of unreacted.
3, a kind of iron mud that produces in the iron powder reducing technology according to claim 1 method of producing iron oxide black as raw material, it is characterized in that: wherein the solid formation B described in step f, the g is that main component is Fe 3O 4Synthetic iron mud.
CNB021159602A 2002-06-11 2002-06-11 Process for preparing iron oxide black from iron sludge generated in iron powder reduction technology Expired - Fee Related CN1160255C (en)

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CN1160255C true CN1160255C (en) 2004-08-04

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Families Citing this family (6)

* Cited by examiner, † Cited by third party
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
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
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
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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