CN105502512A - Method for preparing iron oxide yellow from steel pickling wastewater - Google Patents
Method for preparing iron oxide yellow from steel pickling wastewater Download PDFInfo
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- CN105502512A CN105502512A CN201610084122.2A CN201610084122A CN105502512A CN 105502512 A CN105502512 A CN 105502512A CN 201610084122 A CN201610084122 A CN 201610084122A CN 105502512 A CN105502512 A CN 105502512A
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide (Fe2O3)
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
Abstract
The invention discloses a method for preparing iron oxide yellow from steel pickling wastewater. The method includes the following steps that 1, steel pickling wastewater is taken, and a reducing agent is added; 2, the pH is adjusted while stirring is conducted, an auxiliary agent is added, a reaction is conducted for 0.5-3 hours, the mixture stands still and is filtered, and a solution obtained after secondary purification treatment is obtained; 3, a small part of the solution obtained in step 2 is taken and diluted with water, the pH is adjusted, air is introduced while stirring is conducted, and liquid containing iron oxide yellow seed crystals is obtained; 4, water is added to the remaining solution obtained in step 2 while stirring is conducted, air is introduced for oxidation, drying is conducted, and the iron oxide yellow is obtained. According to the method, the steel pickling wastewater is treated, the acid liquor with impurities removed serves as the raw material, the iron oxide yellow which can be used for multiple purposes is obtained, recycling utilization of iron and steel acid pickle is achieved, waste is changed to valuable things, the method is easy to operate and low in cost, the whole process is environmentally friendly, and it is convenient to achieve industrialization.
Description
Technical field
The present invention relates to a kind of method being prepared iron oxide yellow by iron and steel pickling waste liquid.
Background technology
As everyone knows, pickling is requisite process for treating surface in pickling iron and steel process, the zone of oxidation of the method removing steel surface of this technology chemistry.Containing a large amount of ferrous salts and remnants acid in spent acid solution after pickling, if do not add process just directly discharge, iron and steel pickling waste liquid causes huge harm by environment.Have been reported in the literature the treatment technology of pickling iron and steel spent acid solution, but the operation condition of these treatment processs is harsh, complex process, cost is high, is difficult to realize industrialization.Therefore, find a kind of effective means to recycle material that pickling iron and steel spent acid solution makes it to be converted into high added value will be the task that we one of facing is urgent.
Iron oxide yellow is a kind of general iron oxide material of having many uses, because iron oxide yellow has high tinting strength, very strong photostabilization, temperature tolerance, can protect ultraviosensitive material, is that conventional pigment is incomparable.The performance of these excellences of iron oxide yellow, makes it be obtained in many fields such as superior automobile finish paint, woodwork coating, transparent plastics and applies widely.Current, the iron oxide pigment variety that China produces is single, lacks characteristic, added value of product is low, be difficult to take the course of its own in the market competition of fierceness, therefore explore new synthetic route, the quality and the class that improve product will be a major challenge that developing ability of ferrous oxide industry faces.
Along with in world wide to the attention of global ecological environment, Sustainable development and the development of new and high technology to the needs of synthetic materials, from secondary resource, obtain raw material prepare iron oxide yellow and also will become a focus of future studies.If the recycling of Industry Waste by product can be promoted in China, the unmanageable difficult problem of spent acid solution that current steel industry faces can not only be solved, turn waste into wealth, simultaneously also for the development of iron oxide yellow provides more wide prospect.
Summary of the invention
The difficult problem that a large amount of spent pickle liquors that the object of the invention is to face to solve current steel industry cannot process, provides a kind of method being prepared iron oxide yellow by iron and steel pickling waste liquid.
Technical scheme of the present invention is summarized as follows:
Prepared a method for iron oxide yellow by iron and steel pickling waste liquid, comprise the steps:
(1) pre-treatment of iron and steel pickling waste liquid: get iron and steel pickling waste liquid, add reductive agent reduction ferric iron, make mass content be 0.2% ~ 1%, stir, place 8 ?14h;
(2) secondary-cleaned process: under agitation, regulates pH=4 ~ 8 of pretreated iron and steel pickling waste liquid with alkali, add auxiliary agent and make final concentration be 45 ~ 70mg/l, at 40 ~ 80 DEG C, reaction 0.5-3h, leaves standstill, filters, obtain the solution after secondary-cleaned process, survey Fe in solution
2+concentration, and by volume for 1-4:6-9 is divided into two portions;
(3) preparation of iron oxide yellow crystal seed: get the solution that small part step (2) obtains, dilute with water makes Fe
2+=0.2 ~ 0.6mol/l, regulates pH=5.5 ~ 8.5, at 5 ~ 40 DEG C, under 100-400rpm stirs, with flow for 0.05 ~ 0.2m
3/ h passes into air, is oxidizing to pH=3 ~ 6 of solution, must contain the liquid of iron oxide yellow crystal seed;
(4) preparation of iron oxide yellow: under agitation, adds water the solution that remaining most of step (2) obtains and makes Fe
2+concentration be that 0.1 ~ 0.8mol/l obtains solution one, solution one to be joined in the liquid containing iron oxide yellow crystal seed to obtain solution two, makes Fe in the liquid containing iron oxide yellow crystal seed
2+mole number accounts for Fe in solution two
2+10% ~ 50% of mole number, regulates temperature to be 60 ~ 95 DEG C, under the condition of pH=2.0 ~ 4.0, with flow for 0.01 ~ 0.2m
3/ h blowing air oxidation 4 ~ 20h, dry iron oxide yellow.
Described reductive agent is iron powder or scrap iron skin.
Step (1) described mass content is 0.3% ~ 0.5%.
Step (2) secondary-cleaned is treated to: pH=5 ~ 7 regulating pretreated iron and steel pickling waste liquid with alkali, adds auxiliary agent and makes final concentration be 50 ~ 65mg/l, at 50 ~ 65 DEG C, reaction 0.5-3h, leave standstill, filter, obtain the solution after secondary-cleaned process, survey Fe in solution
2+concentration.
Described alkali is sodium hydroxide, ammoniacal liquor, sodium carbonate or sodium bicarbonate.
Described auxiliary agent is polyacrylamide or poly-iron chloride.
Being prepared as of step (3) iron oxide yellow crystal seed: get the solution that small part step (2) obtains, dilute with water makes Fe
2+=0.2 ~ 0.6mol/l, regulates pH=6.0 ~ 8.0, at 10 ~ 30 DEG C, under 200-400rpm stirs, with flow for 0.08 ~ 0.15m
3/ h passes into air, is oxidizing to pH=4 ~ 6 of solution, must contain the liquid of iron oxide yellow crystal seed.
Being prepared as of step (4) iron oxide yellow: under agitation, adds water the solution that remaining most of step (2) obtains and makes Fe
2+concentration be that 0.2 ~ 0.8mol/l obtains solution one, solution one to be joined in the liquid containing iron oxide yellow crystal seed to obtain solution two, makes Fe in the liquid containing iron oxide yellow crystal seed
2+mole number accounts for Fe in solution two
2+25% ~ 40% of mole number, regulates temperature to be 75 ~ 90 DEG C, under the condition of pH=2.0 ~ 4.0, with flow for 0.08 ~ 0.15m
3/ h blowing air oxidation 6 ~ 16h, dry iron oxide yellow.
Advantage of the present invention: the present invention adopts a kind of easy impurity removal process to process iron and steel pickling waste liquid, obtain the iron content acid solution that clear foreign matter content is low, and with the acid solution after removal of impurities for raw material, obtain versatile iron oxide yellow, achieve the recycling of iron and steel spent acid solution, turn waste into wealth, in active response world wide, environmental protection obtains higher economic benefit while calling, and the unmanageable difficult problem of spent pickle liquor faced for steel industry provides a kind of solution.Method of the present invention is simple to operate, and cost is low, and whole process environmental protection, is convenient to realize industrialization.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the iron oxide yellow that embodiment 2 obtains.
Fig. 2 is the TEM figure of the iron oxide yellow that embodiment 2 obtains.
Fig. 3 is the SEM figure of the iron oxide yellow that embodiment 2 obtains.
Fig. 4 is the XRD figure of the iron oxide yellow that embodiment 5 obtains.
Fig. 5 is the TEM figure of the iron oxide yellow that embodiment 5 obtains.
Fig. 6 is the SEM figure of the iron oxide yellow that embodiment 5 obtains.
Embodiment
Below in conjunction with concrete example, the present invention is described further, and example below better understands the present invention to enable those skilled in the art to, but do not impose any restrictions the present invention.
Embodiment 1
Prepared a method for iron oxide yellow by iron and steel pickling waste liquid, comprise the steps:
(1) pre-treatment of iron and steel pickling waste liquid: get iron and steel pickling waste liquid, adds scrap iron skin, makes mass content be 0.3%, stirs, and places 14h;
(2) secondary-cleaned process: under agitation, the pH=5 of pretreated iron and steel pickling waste liquid is regulated with sodium hydroxide solution, adding polyacrylamide makes final concentration be 45mg/l, at 40 DEG C, reaction 1h, cooling, standing, filtration, obtain the solution after secondary-cleaned process, with the Fe in potassium bichromate solution volumetric solution
2+concentration is n (Fe
2+)=1.923mol/l;
By the solution 345ml after secondary-cleaned process by volume for 3:7 is divided into two portions;
(3) preparation of iron oxide yellow crystal seed: get the solution that small part (3 parts) step (2) obtains, dilute with water makes Fe
2+=0.3mol/l, regulates pH=6.0 with ammoniacal liquor, at 30 DEG C, under 400rpm stirs, take flow as 0.08m
3/ h passes into air, is oxidizing to the pH=4 of solution, obtains the liquid containing iron oxide yellow crystal seed;
(4) preparation of iron oxide yellow: under agitation, adds water the solution that major part (7 parts) step (2) obtains and makes Fe
2+concentration be that 0.3mol/l obtains solution one, solution one to be joined in the liquid containing iron oxide yellow crystal seed to obtain solution two, makes Fe in the liquid containing iron oxide seed crystal
2+mole number accounts for Fe in solution two
2+10% of mole number, is warming up to 95 DEG C, under controlling the pH=3.0 condition of solution, take flow as 0.08m with weak ammonia
3/ h blowing air oxidation 6h, dry iron oxide yellow 39.4g;
Embodiment 2
Prepared a method for iron oxide yellow by iron and steel pickling waste liquid, comprise the steps:
1) pre-treatment of iron and steel pickling waste liquid: get iron and steel pickling waste liquid, add reduced iron powder, makes mass content be 0.2%, stirs, and places 8h;
2) secondary-cleaned process: under agitation, the pH=7 of pretreated iron and steel pickling waste liquid is regulated with aqueous sodium carbonate, adding polyacrylamide makes final concentration be 50mg/l, at 50 DEG C, reaction 0.5h, cooling, standing, filtration, obtain the solution after secondary-cleaned process, with the Fe in potassium bichromate solution volumetric solution
2+concentration is n (Fe
2+)=1.998mol/l;
By the solution 180ml after secondary-cleaned process by volume for 4:6 is divided into two portions
(3) preparation of iron oxide yellow crystal seed: get the solution that small part (4 parts) step (2) obtains, dilute with water makes Fe
2+=0.2mol/l, regulates pH=8.0 with sodium hydroxide solution, at 10 DEG C, under 200rpm stirs, take flow as 0.15m
3/ h passes into air, is oxidizing to the pH=4 of solution, obtains the liquid containing iron oxide yellow crystal seed;
(4) preparation of iron oxide yellow: under agitation, adds water the solution that remaining major part (6 parts) step (2) obtains and makes Fe
2+concentration be that 0.2mol/l obtains solution one, solution one to be joined in the liquid containing iron oxide yellow crystal seed to obtain solution two, makes Fe in the liquid containing iron oxide yellow crystal seed
2+mole number accounts for Fe in solution two
2+25% of mole number, is warming up to 75 DEG C, under pH=2.5 condition, take flow as 0.15m
3/ h blowing air oxidation 16h obtains iron oxide yellow 20.8g.
Embodiment 3
Prepared a method for iron oxide yellow by iron and steel pickling waste liquid, comprise the steps:
(1) pre-treatment of iron and steel pickling waste liquid: get iron and steel pickling waste liquid, adds reductive agent iron powder, makes mass content be 1%, stirs, and places 12h;
(2) secondary-cleaned process: under agitation, the pH=8 of pretreated iron and steel pickling waste liquid is regulated with sodium bicarbonate aqueous solution, adding polyacrylamide makes final concentration be 65mg/l, at 65 DEG C, reaction 3h, cooling, standing, filtration, obtain the solution after secondary-cleaned process, with the Fe in potassium bichromate solution volumetric solution
2+concentration is n (Fe
2+)=2.058mol/l;
By the solution 350ml after secondary-cleaned process by volume for 4:6 is divided into two portions;
(3) preparation of iron oxide yellow crystal seed: get the solution that small part (4 parts) step (2) obtains, dilute with water makes Fe
2+=0.6mol/l, regulates pH=5.5 with ammoniacal liquor, at 5 DEG C, under 300rpm stirs, take flow as 0.2m
3/ h passes into air, is oxidizing to the pH=6 of solution, obtains the liquid containing iron oxide yellow crystal seed;
(4) preparation of iron oxide yellow: under agitation, adds water the solution that remaining major part (6 parts) step (2) obtains and makes Fe
2+concentration be that 0.8mol/l obtains solution one, solution one to be joined in the liquid containing iron oxide yellow crystal seed to obtain solution two, makes Fe in the liquid containing iron oxide yellow crystal seed
2+mole number accounts for Fe in solution two
2+40% of mole number, is warming up to 90 DEG C, under pH=4 condition, take flow as 0.01m
3/ h blowing air is oxidizing to 20h, dry iron oxide yellow 43.5g.
Embodiment 4
Prepared a method for iron oxide yellow by iron and steel pickling waste liquid, comprise the steps:
(1) pre-treatment of iron and steel pickling waste liquid: get iron and steel pickling waste liquid, adds reductive agent scrap iron skin, makes mass content be 0.2%, stirs, and places 13h;
(2) secondary-cleaned process: under agitation, the pH=4 of pretreated iron and steel pickling waste liquid is regulated with aqueous sodium hydroxide solution, adding poly-iron chloride makes final concentration be 70mg/l, at 80 DEG C, reaction 2h, cooling, standing, filtration, obtain the solution after secondary-cleaned process, with the Fe in potassium bichromate solution volumetric solution
2+concentration is n (Fe
2+)=1.913mol/l;
By the solution 262ml after secondary-cleaned process by volume for 1:9 is divided into two portions
(3) preparation of iron oxide yellow crystal seed: get the solution that small part (1 part) step (2) obtains, dilute with water makes Fe
2+=0.5mol/l, regulates pH=8.5 with ammoniacal liquor, at 40 DEG C, under 100rpm stirs, take flow as 0.05m
3/ h passes into air, is oxidizing to the pH=3 of solution, obtains the liquid containing iron oxide yellow crystal seed;
(4) preparation of iron oxide yellow: under agitation, adds water the solution that remaining major part (9 parts) step (2) obtains and makes Fe
2+concentration be that 0.1mol/l obtains solution one, solution one to be joined in the liquid containing iron oxide yellow crystal seed to obtain solution two, makes Fe in the liquid containing iron oxide yellow crystal seed
2+mole number accounts for Fe in solution two
2+50% of mole number, is warming up to 60 DEG C, under pH=2 condition, take flow as 0.2m
3/ h blowing air oxidation 4h, dry iron oxide yellow 35.6g;
Embodiment 5
Prepared a method for iron oxide yellow by iron and steel pickling waste liquid, comprise the steps:
(1) pre-treatment of iron and steel pickling waste liquid: get iron and steel pickling waste liquid, add reduced iron powder, makes mass content be 0.5%, stirs, and places 11h;
(2) removal of impurities: under agitation, the pH=5.5 of pretreated iron and steel pickling waste liquid is regulated with weak ammonia, adding polyacrylamide makes final concentration be 65mg/l, at 60 DEG C, reaction 2.5h, cooling, standing, filtration, obtain the solution after secondary-cleaned process, with the Fe in potassium bichromate solution volumetric solution
2+concentration is n (Fe
2+)=2.043mol/l;
By the solution 399ml after secondary-cleaned process by volume for 2:8 is divided into two portions
(3) preparation of iron oxide yellow crystal seed: get the solution that small part (2 parts) step (2) obtains, dilute with water makes Fe
2+=0.5mol/l, regulates pH=7.5 with ammoniacal liquor, at 30 DEG C, under 300rpm stirs, take flow as 0.14m
3/ h passes into air, is oxidizing to the pH=6 of solution, obtains the liquid containing iron oxide yellow crystal seed;
(4) preparation of iron oxide yellow: under agitation, adds water the solution that remaining major part (8 parts) step (2) obtains and makes Fe
2+concentration be that 0.4mol/l obtains solution one, solution one to be joined in the liquid containing iron oxide yellow crystal seed to obtain solution two, makes Fe in the liquid containing iron oxide yellow crystal seed
2+mole number accounts for Fe in solution two
2+28% of mole number, is warming up to 90 DEG C, under pH=6.5 condition, take flow as 0.15m
3/ h blowing air is oxidizing to 7h and obtains iron oxide yellow 52.5g.
Claims (8)
1. prepared a method for iron oxide yellow by iron and steel pickling waste liquid, it is characterized in that comprising the steps:
(1) pre-treatment of iron and steel pickling waste liquid: get iron and steel pickling waste liquid, add reductive agent reduction ferric iron, make mass content be 0.2% ~ 1%, stir, place 8 ?14h;
(2) secondary-cleaned process: under agitation, regulates pH=4 ~ 8 of pretreated iron and steel pickling waste liquid with alkali, add auxiliary agent and make final concentration be 45 ~ 70mg/l, at 40 ~ 80 DEG C, reaction 0.5-3h, leaves standstill, filters, obtain the solution after secondary-cleaned process, survey Fe in solution
2+concentration, and by volume for 1-4:6-9 is divided into two portions;
(3) preparation of iron oxide yellow crystal seed: get the solution that small part step (2) obtains, dilute with water makes Fe
2+=0.2 ~ 0.6mol/l, regulates pH=5.5 ~ 8.5, at 5 ~ 40 DEG C, under 100-400rpm stirs, with flow for 0.05 ~ 0.2m
3/ h passes into air, is oxidizing to pH=3 ~ 6 of solution, must contain the liquid of iron oxide yellow crystal seed;
(4) preparation of iron oxide yellow: under agitation, adds water the solution that remaining most of step (2) obtains and makes Fe
2+concentration be that 0.1 ~ 0.8mol/l obtains solution one, solution one to be joined in the liquid containing iron oxide yellow crystal seed to obtain solution two, makes Fe in the liquid containing iron oxide yellow crystal seed
2+mole number accounts for Fe in solution two
2+10% ~ 50% of mole number, regulates temperature to be 60 ~ 95 DEG C, under the condition of pH=2.0 ~ 4.0, with flow for 0.01 ~ 0.2m
3/ h blowing air oxidation 4 ~ 20h, dry iron oxide yellow.
2. method according to claim 1, is characterized in that described reductive agent is iron powder or scrap iron skin.
3. method according to claim 1 and 2, is characterized in that step (1) described mass content is 0.3% ~ 0.5%.
4. method according to claim 1, it is characterized in that described step (2) secondary-cleaned is treated to: pH=5 ~ 7 regulating pretreated iron and steel pickling waste liquid with alkali, adding auxiliary agent makes final concentration be 50 ~ 65mg/l, at 50 ~ 65 DEG C, reaction 0.5-3h, leave standstill, filter, obtain the solution after secondary-cleaned process, survey Fe in solution
2+concentration.
5. the method according to claim 1 or 4, is characterized in that described alkali is sodium hydroxide, ammoniacal liquor, sodium carbonate or sodium bicarbonate.
6. the method according to claim 1 or 4, is characterized in that described auxiliary agent is polyacrylamide or poly-iron chloride.
7. method according to claim 1, is characterized in that being prepared as of step (3) iron oxide yellow crystal seed: get the solution that small part step (2) obtains, dilute with water makes Fe
2+=0.2 ~ 0.6mol/l, regulates pH=6.0 ~ 8.0, at 10 ~ 30 DEG C, under 200-400rpm stirs, with flow for 0.08 ~ 0.15m
3/ h passes into air, is oxidizing to pH=4 ~ 6 of solution, must contain the liquid of iron oxide yellow crystal seed.
8. method according to claim 1, is characterized in that being prepared as of step (4) iron oxide yellow: under agitation, and being added water by the solution that remaining most of step (2) obtains makes Fe
2+concentration be that 0.2 ~ 0.8mol/l obtains solution one, solution one to be joined in the liquid containing iron oxide yellow crystal seed to obtain solution two, to make in solution two Fe in iron oxide yellow crystal seed
2+content account for total Fe in solution two
2+25% ~ 40% of content, regulates temperature to be 75 ~ 90 DEG C, under the condition of pH=2.0 ~ 4.0, with flow for 0.08 ~ 0.15m
3/ h blowing air oxidation 6 ~ 16h, dry iron oxide yellow.
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| CN107585791A (en) * | 2017-09-28 | 2018-01-16 | 福州琪宁精细化工有限公司 | A kind of preparation method of iron oxide |
| CN108455681A (en) * | 2018-02-05 | 2018-08-28 | 吉林建筑大学 | A method of preparing iron oxide yellow using iron content, aluminum i ndustry waste water |
| CN108640159A (en) * | 2018-02-27 | 2018-10-12 | 天津丹兴科技有限责任公司 | A kind of pickling sludge and pickle liquor harmless resource utilization integrated conduct method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107585791A (en) * | 2017-09-28 | 2018-01-16 | 福州琪宁精细化工有限公司 | A kind of preparation method of iron oxide |
| CN108455681A (en) * | 2018-02-05 | 2018-08-28 | 吉林建筑大学 | A method of preparing iron oxide yellow using iron content, aluminum i ndustry waste water |
| CN108640159A (en) * | 2018-02-27 | 2018-10-12 | 天津丹兴科技有限责任公司 | A kind of pickling sludge and pickle liquor harmless resource utilization integrated conduct method |
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|---|---|
| CN105502512B (en) | 2017-06-20 |
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