CN107381654A - A kind of method that liquid industrial frerrous chloride is converted into by hydrochloric acid pickling waste liquor - Google Patents
A kind of method that liquid industrial frerrous chloride is converted into by hydrochloric acid pickling waste liquor Download PDFInfo
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- CN107381654A CN107381654A CN201710833444.7A CN201710833444A CN107381654A CN 107381654 A CN107381654 A CN 107381654A CN 201710833444 A CN201710833444 A CN 201710833444A CN 107381654 A CN107381654 A CN 107381654A
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- hydrochloric acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/10—Halides
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Abstract
The invention discloses a kind of method that liquid industrial frerrous chloride is converted into by hydrochloric acid pickling waste liquor, step：(1) hydrochloric acid pickling waste liquor is subjected to constituent analysis；(2) iron scale is added in hydrochloric acid pickling waste liquor, stirring, adds reducing agent, stirring；(3) filter, filtrate is liquid industrial frerrous chloride, and obtained filter residue contains iron scale and reducing agent, and reuse is added after next reactions steps (2) add iron scale.Hydrochloric acid pickling waste liquor and iron scale that the present invention uses are the discarded object of Steel-rolling Industry, produce liquid industrial frerrous chloride as raw material, have not only solved problem of environmental pollution but also generated economic benefit.This method spent acid treating capacity is big simultaneously, and technique is simple, avoids regenerated acid reuse difficult, obtained product frerrous chloride content >=20wt%, free acid content≤0.5wt%, meet standard HG/T 4,200 2011, chlorinating agent, flocculant, decolorising agent etc. can be used as to be used for other industry.
Description
Technical field
The present invention relates to a kind of spent acid processing method, more particularly to one kind is converted into liquid industrial chlorine by hydrochloric acid pickling waste liquor
Change ferrous method, belong to industrial dangerous waste resource recycling and utilize field.
Background technology
Steel plate is the important raw and processed materials of auto industry, household electrical appliance, Container Transport and Welded tube production industry.Due to putting
The surface of steel plate put too long often forms one layer of iron scale, therefore is required for removing this layer through overpickling before cold-rolling of steel plate
Iron scale, substantial amounts of hydrochloric acid will be so consumed, so as to generate substantial amounts of waste hydrochloric acid.With a middle-size and small-size cold rolling
Exemplified by factory, its daily up to tens of to up to a hundred ton of spent acid amount.In general, in the spent acid of cold rolling mill output free hydrochloric acid content
About 1wt/%~16wt/%, frerrous chloride content>10wt/%.The method of the spent acid of processing cold rolling mill output mainly has at present
Neutralisation, roasting method, evaporation, sulfate substitution method etc..
Neutralisation is until reaching and can directly be discharged after discharge standard using substantial amounts of lime with hydrochloric acid reaction.This method exists
Consume large quantities of lime simultaneously, also result in the waste of the hydrochloric acid and frerrous chloride in a large amount of spent acid.Fe contained in waste liquid after discharge2+
It is oxidized to Fe3+After water body is changed into brown, cause soil hardening, have a strong impact on ecological environment.Therefore, neutralisation is a kind of dirty
The method of thing transfer is contaminated, is only applicable to handle a small amount of pickle liquor.
Roasting method is by the hydrochloric acid in high-temperature roasting waste acid recovery, while generation such as iron chloride or ferric oxide particles.Should
Method mainly has spray roasting and fluosolids roasting method.Spray roasting is by the way that spent acid is sprayed by the nozzle of roast furnace top
Enter in stove, put the direct-fired mode of coal gas in burner, finally spray obtains hydrochloric acid of living again from tail gas, and furnace bottom obtains iron oxide
Particle.The sintering temperature of this method is typically at 600~800 DEG C.Sulfidation roasting is that spent acid is sprayed into the flowing molten iron medium containing oxidation
In fluid bed, coal gas lights heating by bottom, finally gives live again hydrochloric acid and ferric oxide particles.This method advantage is that hydrochloric acid returns
Yield is big, concentration is high, and the concentration of hydrochloric acid of recovery is 20% or so；Shortcoming is that investment is high, including floor space is big, equipment investment
It is high, operating cost is high, civil engineering, complex structural designs, includes the supply of thermal source, cooling water, the pickling effect of hydrochloric acid of living again is poor,
Use difficulty.Gained ferric oxide particles impurity quality is big simultaneously, and purity is not high to cause price low.Due to its so high input and
Energy consumption, it is merely capable of being used among large-scale pickling unit at present.
Evaporation is to evaporate spent acid under subnormal ambient, and hydrochloric acid and water are evaporated from spent acid, is reclaimed by cooling
Hydrochloric acid.Gained concentrate crystallisation by cooling, about 22% or so hydrochloric acid and frerrous chloride crystal are finally given after separation of solid and liquid, should
Method advantage is：The investment of civil engineering and equipment is smaller, without very complicated structure.But its production cycle is longer, treating capacity is not
Greatly, and gained concentrated mother liquor is needed to return after separation of solid and liquid and distilled, and energy consumption (steam, electricity etc.) is higher, is suitable for steel wire, steel pipe
And the less small-sized pickling unit of the spent acid amount such as steel tower.
Sulfate substitution method is to be based on evaporation, and the concentration of hydrochloric acid obtained by evaporation is relatively low, therefore is added in spent acid
Enter sulfuric acid, sulfuric acid and frerrous chloride occur displacement reaction, finally give ferrous sulfate and hydrochloric acid.Afterwards by negative pressure evaporation,
Separation of solid and liquid obtains the higher hydrochloric acid of concentration and errous sulfate crystal.Concentration of hydrochloric acid obtained by this method is higher, while obtains sulfuric acid
It is ferrous.But it is complete reaction between ions, therefore hydrochloric acid and sulphur be present simultaneously in gained acid solution because the reaction is displacement reaction
Sour ferrous, separating difficulty is larger.Simultaneously because ferrous sulfate is DDGS, its solubility is 66.67g, and therefore, separation has certain
Difficulty, cause gained hydrochloric acid concentration be less than theoretical concentration.If excess sulfuric acid, a certain amount of sulphur can be contained in recovery acid
Acid, i.e., usually obtain nitration mixture, severe corrosion equipment.Further, since adding sulfuric acid, cost is caused also accordingly to increase, also can shadow
Ring benefit.
Spent acid processing method described above has that spent acid treating capacity is small, cost of investment is high, high energy consumption, caused regenerated acid make
The problems such as with difficulty and bad pickling effect.For this problem, patent CN104229902A proposes a kind of using waste hydrochloric acid as original
Material prepares the water process ferrous method of liquid chlorine, but this method need hydrochloric acid to being used in steel rolling acid cleaning process and
Frerrous chloride and free acid content are controlled in caused waste hydrochloric acid, not only increase the complexity of acid cleaning process and to
Through generating frerrous chloride content<20%wt%, free acid content>5wt% waste hydrochloric acid does not apply to.However, often due to production
Purposes is different with technique, frerrous chloride content in waste hydrochloric acid caused by enterprise's presence<20%wt%, free acid content>5wt%.
Spent acid belongs to one of three industrial wastes, will certainly be to surrounding environment if arbitrarily stacking if unreasonable disposal or recycling
Serious pollution is caused, while valuable metal can not be reclaimed, is a kind of wasting of resources.Therefore, a kind of green of exploitation, environment friend
Good, simple to operate, Eco-power method realizes recycling for a large amount of waste acid resources, is cold-rolled steel sheet industry is urgently to be resolved hurrily
Problem.
The content of the invention
The purpose of the present invention is overcome the deficiencies in the prior art, there is provided a kind of spent acid treating capacity is big, simple to operate, production week
Phase is short, cost of investment is low, avoids regenerated acid from Steel-rolling Industry discarded object being carried out into resource recycling using difficulty, both be solved
Certainly problem of environmental pollution creates a kind of method that liquid industrial frerrous chloride is converted into by hydrochloric acid pickling waste liquor of economic benefit again.
Technical scheme is summarized as follows：
A kind of method that liquid industrial frerrous chloride is converted into by hydrochloric acid pickling waste liquor, comprises the following steps：
(1) hydrochloric acid pickling waste liquor is subjected to constituent analysis, frerrous chloride content in hydrochloric acid pickling waste liquor>10wt/%, hydrochloric acid
Free acid content in pickle liquor in terms of HCl is in 1wt/%~16wt/% scopes；Particularly 1.21wt/%~
15.88wt/%；
(2) iron scale is added in hydrochloric acid pickling waste liquor, at 20-60 DEG C, stirs 10~30min, add reducing agent,
At 20-60 DEG C, 10~40min is stirred；
The iron scale is the 0.5%~8% of hydrochloric acid pickling waste liquor quality；The quality of the reducing agent and iron scale
Than for 1:(2~5)；
(3) liquid that step (2) obtains is separated by filtration, obtained filtrate is liquid industrial frerrous chloride, is obtained
Filter residue contains iron scale and reducing agent, and reuse is added after the addition iron scale of next reactions steps (2).
Preferentially, iron scale is the 2%~4% of hydrochloric acid pickling waste liquor quality.
Preferentially, the mass ratio of reducing agent and iron scale is 1:3.
Preferentially, reducing agent is reduced iron powder or pig iron powder.
Preferentially, the speed of step (2) stirring is 20~200r/min.
Advantages of the present invention：
(1) hydrochloric acid pickling waste liquor used in the inventive method and iron scale are the discarded object of Steel-rolling Industry, by it
Liquid industrial frerrous chloride is produced as raw material, is turned waste into wealth, has both solved the dirt of the environment such as industrial waste acid, solid waste discharge
Dye problem generates economic benefit again.
(2) the inventive method spent acid treating capacity is big, and reaction condition is gentle, and technique is simple, with short production cycle, cost of investment
It is low, obtained product frerrous chloride content >=20%wt%, free acid content≤0.5wt%, meet standard HG/T 4200-
2011。
(3) hydrochloric acid pickling waste liquor is directly produced as qualified products by the inventive method, avoids existing spent acid handling process from producing
The problems such as raw regenerated acid is using difficult and pickling effect difference.
(4) the liquid industrial frerrous chloride that the inventive method finally gives, can be with addition to as in general industrial application
Directly as chlorinating agent, ferroso-ferric oxide and carbon is coordinated to carry out the collaboration chlorination of polymetallic ore (sulfate slag or lateritic nickel ore etc.)
Roasting, also production raw material are provided for pyrometallurgy while handling spent acid and reclaiming valuable metal.At the same time as wadding
Solidifying agent, decolorising agent etc. are used for other industry.
Embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment.Those skilled in the art will manage
Solution, following examples are only the preferred embodiments of the present invention, in order to more fully understand the present invention, thus should not be regarded as limiting this
The scope of invention.For those skilled in the art, the present invention can have various modifications and variations, all essences in the present invention
God any modification, equivalent substitution or improvement for being made etc., should be included in the scope of the protection with principle.
Experimental method in following embodiments, it is conventional method unless otherwise specified；Experiment material used, such as nothing
Specified otherwise, it is available from commercially available from routine biochemistry chemical reagent work.
Embodiment 1
A kind of method that liquid industrial frerrous chloride is converted into by hydrochloric acid pickling waste liquor, comprises the following steps：
(1) hydrochloric acid pickling waste liquor is subjected to constituent analysis, frerrous chloride content=32.90wt/% in hydrochloric acid pickling waste liquor；
Free acid content in hydrochloric acid pickling waste liquor in terms of HCl is in 1.21wt/%；
(2) iron scale is added in hydrochloric acid pickling waste liquor, at 50 DEG C, mixing speed 140r/min, stirs 10min,
Reduced iron powder is added, at 20 DEG C, stirs 40min；
The iron scale is the 0.5% of hydrochloric acid pickling waste liquor quality；The mass ratio of the reduced iron powder and iron scale
For 1:5；
(3) liquid that step (2) obtains is separated by filtration, obtained liquid is liquid industrial frerrous chloride, its composition
1 is shown in Table, its product content complies fully with HG/T 4200-2011 liquid industrial frerrous chloride requirements and is shown in Table 1：
Obtained filter residue contains iron scale and reduced iron powder, is added after the addition iron scale of next reactions steps (2)
Reuse.Table 1
Embodiment 2
A kind of method that liquid industrial frerrous chloride is converted into by hydrochloric acid pickling waste liquor, comprises the following steps：
(1) hydrochloric acid pickling waste liquor is subjected to constituent analysis, frerrous chloride content=22.70wt/% in hydrochloric acid pickling waste liquor,
Free acid content in hydrochloric acid pickling waste liquor in terms of HCl is in 3.06wt/%；
(2) iron scale is added in hydrochloric acid pickling waste liquor, at 20 DEG C, mixing speed 80r/min, stirs 30min, then
Reduced iron powder is added, at 20 DEG C, stirs 40min；
The iron scale is the 2% of hydrochloric acid pickling waste liquor quality；The mass ratio of the reduced iron powder and iron scale is
1:3；
(3) liquid that step (2) obtains is separated by filtration, obtained liquid is liquid industrial frerrous chloride, its composition
2 are shown in Table, its product content complies fully with HG/T 4200-2011 liquid industrial frerrous chloride requirements.Obtained filter residue contains iron oxide
Skin and reduced iron powder, reuse is added after the addition iron scale of next reactions steps (2).
Table 2
Embodiment 3
A kind of method that liquid industrial frerrous chloride is converted into by hydrochloric acid pickling waste liquor, comprises the following steps：
(1) hydrochloric acid pickling waste liquor is subjected to constituent analysis, frerrous chloride content=22.70wt/% in hydrochloric acid pickling waste liquor,
Free acid content in hydrochloric acid pickling waste liquor in terms of HCl is in 3.06wt/%；
(2) iron scale is added in hydrochloric acid pickling waste liquor, at 60 DEG C, the speed of stirring is 20r/min, stirs 10min,
Pig iron powder is added, at 60 DEG C, stirs 10min；
The iron scale is the 4% of hydrochloric acid pickling waste liquor quality；The mass ratio of the pig iron powder and iron scale is 1:
3；
(3) liquid that step (2) obtains is separated by filtration, obtained liquid is liquid industrial frerrous chloride, its composition
3 are shown in Table, its product content complies fully with HG/T 4200-2011 liquid industrial frerrous chloride requirements.Obtained filter residue contains iron oxide
Skin and pig iron powder, reuse is added after the addition iron scale of next reactions steps (2).
Table 3
Embodiment 4
A kind of method that liquid industrial frerrous chloride is converted into by hydrochloric acid pickling waste liquor, comprises the following steps：
(1) hydrochloric acid pickling waste liquor is subjected to constituent analysis, frerrous chloride content=18.21wt/% in hydrochloric acid pickling waste liquor,
Free acid content in hydrochloric acid pickling waste liquor in terms of HCl is in 5.98wt/%；
(2) iron scale is added in hydrochloric acid pickling waste liquor, at 40 DEG C, mixing speed 140r/min, stirs 28min,
Pig iron powder is added, at 40 DEG C, stirs 33min；
The iron scale is the 8% of hydrochloric acid pickling waste liquor quality；The mass ratio of the pig iron powder and iron scale is 1:
2；
(3) liquid that step (2) obtains is separated by filtration, obtained liquid is liquid industrial frerrous chloride, its composition
4 are shown in Table, its product content complies fully with HG/T 4200-2011 liquid industrial frerrous chloride requirements.Obtained filter residue contains iron oxide
Skin and pig iron powder, reuse is added after the addition iron scale of next reactions steps (2).
Table 4
Embodiment 5
A kind of method that liquid industrial frerrous chloride is converted into by hydrochloric acid pickling waste liquor, comprises the following steps：
(1) hydrochloric acid pickling waste liquor is subjected to constituent analysis, frerrous chloride content=10.01wt/% in hydrochloric acid pickling waste liquor,
Free acid content in hydrochloric acid pickling waste liquor in terms of HCl is in 15.88wt/%；
(2) iron scale is added in hydrochloric acid pickling waste liquor, at 60 DEG C, mixing speed 200r/min, stirs 30min,
Reduced iron powder is added, at 60 DEG C, stirs 33min；
The iron scale is the 8% of hydrochloric acid pickling waste liquor quality；The mass ratio of the reduced iron powder and iron scale is
1:4；
(3) liquid that step (2) obtains is separated by filtration, obtained filter body is liquid industrial frerrous chloride, its composition
5 are shown in Table, its product content complies fully with HG/T 4200-2011 liquid industrial frerrous chloride requirements.Obtained filter residue contains iron oxide
Skin and reduced iron powder, reuse is added after the addition iron scale of next reactions steps (2).
Table 5
For the present invention in acidolysis reduction process, the chemical reaction mainly occurred is as follows：
Fe3O4+8HCl→FeCl2+2FeCl3+4H2O
FeO+2HCl→FeCl2+H2O
Fe2O3+6HCl→2FeCl3+3H2O
Fe+2FeCl3→3FeCl2
Comparative example 1：
In addition to not adding iron scale in step (2), other steps are same as Example 2.
Comparative example 2：
In addition to being not added with pig iron powder in step (2), other steps are same as Example 4.
If integrated embodiment 1-5 and comparative example 1-2 result, which can be seen that, is not added with iron scale and reducing agent, production
Product do not reach liquid industrial frerrous chloride free acid and frerrous chloride content requirement.
The discarded object of Steel-rolling Industry is produced liquid industrial frerrous chloride by the inventive method, both solves environment
Pollution problem generates economic benefit again.This method spent acid treating capacity is big simultaneously, and reaction condition is gentle, and technique is simple, and cost is low,
Obtained product frerrous chloride content >=20wt%, free acid content≤0.5wt%, meets standard HG/T 4200-2011, can
To be used for other industry as chlorinating agent, flocculant, decolorising agent etc..
The present invention illustrates the process of the present invention by above-described embodiment, but the invention is not limited in above-mentioned technique
Step, that is, do not mean that the present invention has to rely on above-mentioned processing step and could implemented.Person of ordinary skill in the field should
Understand, any improvement in the present invention, the addition of equivalence replacement and auxiliary element to raw material selected by the present invention, concrete mode
Selection etc., be within the scope of the present invention.
Claims (5)
- A kind of 1. method that liquid industrial frerrous chloride is converted into by hydrochloric acid pickling waste liquor, it is characterised in that comprise the following steps：(1) hydrochloric acid pickling waste liquor is subjected to constituent analysis, frerrous chloride content in hydrochloric acid pickling waste liquor>10wt/%, chlorohydric acid pickling Free acid content in waste liquid in terms of HCl is in 1wt/%~16wt/% scopes；(2) iron scale is added in hydrochloric acid pickling waste liquor, at 20-60 DEG C, stirs 10~30min, add reducing agent, 20-60 DEG C, stir 10~40min；The iron scale is the 0.5%~8% of hydrochloric acid pickling waste liquor quality；The reducing agent with The mass ratio of iron scale is 1:(2~5)；(3) liquid that step (2) obtains is separated by filtration, obtained filtrate is liquid industrial frerrous chloride, obtained filter residue Containing iron scale and reducing agent, reuse is added after the addition iron scale of next reactions steps (2).
- 2. according to the method for claim 1, it is characterised in that the iron scale for hydrochloric acid pickling waste liquor quality 2%~ 4%.
- 3. according to the method for claim 1, it is characterised in that the mass ratio of the reducing agent and iron scale is 1:3.
- 4. the method according to claim 1 or 3, it is characterised in that the reducing agent is reduced iron powder or pig iron powder.
- 5. according to the method for claim 1, it is characterised in that the speed of step (2) stirring is 20~200r/min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110980833A (en) * | 2019-12-16 | 2020-04-10 | 斯瑞尔环境科技股份有限公司 | Preparation method of electronic-grade ferrous chloride |
| CN111170373A (en) * | 2020-01-07 | 2020-05-19 | 斯瑞尔环境科技股份有限公司 | Preparation method of ferrous chloride tetrahydrate |
| CN114835170A (en) * | 2022-06-06 | 2022-08-02 | 湖南华菱涟钢特种新材料有限公司 | Production process of iron oxide powder with low calcium content |
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| CN105399187A (en) * | 2015-11-20 | 2016-03-16 | 扬州祥发资源综合利用有限公司 | Method for resource utilization of steel wire rope pickling waste liquor |
| CN105696010A (en) * | 2016-01-12 | 2016-06-22 | 惠州市斯瑞尔环境化工有限公司 | Method for recycling iron and zinc containing waste hydrochloric acid solution |
| CN106745193A (en) * | 2016-12-09 | 2017-05-31 | 东北大学 | The method that iron content zinc-containing sludge recovery prepares zinc hydroxide and dyestuff level iron oxide red |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104828995A (en) * | 2015-05-20 | 2015-08-12 | 中冶东方工程技术有限公司 | Treatment method of ferrous waste hydrochloric acid |
| CN105399187A (en) * | 2015-11-20 | 2016-03-16 | 扬州祥发资源综合利用有限公司 | Method for resource utilization of steel wire rope pickling waste liquor |
| CN105696010A (en) * | 2016-01-12 | 2016-06-22 | 惠州市斯瑞尔环境化工有限公司 | Method for recycling iron and zinc containing waste hydrochloric acid solution |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110980833A (en) * | 2019-12-16 | 2020-04-10 | 斯瑞尔环境科技股份有限公司 | Preparation method of electronic-grade ferrous chloride |
| CN111170373A (en) * | 2020-01-07 | 2020-05-19 | 斯瑞尔环境科技股份有限公司 | Preparation method of ferrous chloride tetrahydrate |
| CN114835170A (en) * | 2022-06-06 | 2022-08-02 | 湖南华菱涟钢特种新材料有限公司 | Production process of iron oxide powder with low calcium content |
| CN114835170B (en) * | 2022-06-06 | 2023-11-28 | 湖南华菱涟钢特种新材料有限公司 | Production process of low-calcium-content ferric oxide powder |
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Application publication date: 20171124 |