CN104478001A - Method for producing iron oxide yellow from acidic waste water in titanium dioxide industry - Google Patents
Method for producing iron oxide yellow from acidic waste water in titanium dioxide industry Download PDFInfo
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- CN104478001A CN104478001A CN201410666586.5A CN201410666586A CN104478001A CN 104478001 A CN104478001 A CN 104478001A CN 201410666586 A CN201410666586 A CN 201410666586A CN 104478001 A CN104478001 A CN 104478001A
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Abstract
The invention relates to a method for producing iron oxide yellow from acidic waste water in titanium dioxide industry. The method comprises the following steps: discharging the raw material acidic waste water into a reaction tank; adding an iron sheet and/or iron powder into the reaction tank; dosing calcium oxide powder into the reaction tank; discharging a solution after the reaction into a filter press for pressure filtration so as to obtain ferrous sulfate waste water and calcium sulfate waste residue after pressure filtration; and discharging the ferrous sulfate waste water into an iron yellow seed crystal tank, measuring and dosing lye into the iron yellow seed crystal tank, controlling the pH value at 3.0-4.0, blowing air into the solution and oxidizing to prepare iron yellow seed crystals; putting an iron yellow seed crystal solution into an oxidation tank, adding the iron sheet and/or iron powder into the oxidation tank, quantitatively adding a ferrous sulfate solution into the solution, and introducing air to oxidize ferrous oxide ions to obtain iron ions till the end of oxidation reaction; and discharging a prepared iron oxide yellow solution into the filter press to obtain finished iron oxide yellow powder, packaging and warehousing. According to the method provided by the invention, harmless treatment of the acidic waste water produced in the titanium dioxide industry is realized, and resources are further recycled.
Description
Technical field
The present invention relates to the production technique of iron oxide yellow, especially a kind of titanium dioxide industry acid waste water produces the method for iron oxide yellow.
Background technology
Ferric oxide, chemical name Fe
2o
3, also known as iron oxide yellow, for various pigment coloration and Protective substances, the method for producing iron oxide yellow is both at home and abroad more, mainly contains green vitriol calcination method, liquid-phase precipitation method, bag core method etc.
Titanium powder plant adopts Production By Sulfuric Acid Process titanium dioxide pigment, is be (FeTiO with ilmenite
3) be raw material, use sulfuric acid decomposition ore, titanium and iron all become vitriol and dissolve, and after completing production titanium dioxide pigment major product and the ferrous by-product of reclaim(ed) sulfuric acid, still have a large amount of acid waste water containing ferrous sulfate to discharge.In this acid waste water, sulfur acid ferrous iron (FeSO
47H
2o) about 20% (200g/L), sulfuric acid are about 15-20% (average 18%), and other impurity is no more than 1.0% as Ti, Mn, Mg, Al etc.Acid waste water can not directly discharge, and pollutes the environment, and containing more useful matter.Acid waste water needs first to carry out pre-treatment ability further extraction useful matter wherein, and after carrying out pre-treatment, obtain a large amount of copperas solutions, ferrous sulfate has higher value, can be used for preparing iron oxide yellow.
Summary of the invention
The technical problem to be solved in the present invention is: provide a kind of titanium dioxide industry acid waste water to produce the method for iron oxide yellow, achieve the nuisanceless disposal of the acid waste water that titanium dioxide industry is produced, resource utilization is recycled.
The technical solution adopted for the present invention to solve the technical problems is: a kind of titanium dioxide industry acid waste water produces the method for iron oxide yellow, has following steps:
1. the raw material acid waste water containing ferrous sulfate and sulfuric acid is entered reactive tank;
2. in reactive tank, add iron sheet and/or iron powder, in reactive tank, pass into steam, acid waste water is heated, promote that iron sheet and/or iron powder and sulfuric acid carry out Fe+H
2sO
4→ FeSO
4+ H
2↑ reaction, produces more ferrous sulfate;
3. after question response for some time, in reactive tank, add lime powder, and CaO+H is carried out in stirring
2sO
4→ CaSO
4+ H
2o neutralization reaction, make the remaining sulfuric acid in acid waste water generate calcium sulfate precipitation thing, the pH value to reactive tank inner acidic waste water reaches 3-4 and namely stops adding lime powder;
4. after reaction being completed, solution enters pressure filter and carries out press filtration, obtain ferrous sulfate waste water and calcium sulfate waste residues after press filtration, the ferrous sulfate waste water after press filtration is entered purification tank for liquid waste, the calcium sulfate waste residues after press filtration enters oven for drying, waste residue after drying is pulverized, makes calcium sulphate powders;
5. the ferrous sulfate waste water in purification tank for liquid waste is entered iron oxide seed crystal tank, in iron oxide seed crystal tank, metering adds alkali lye, and generate ferrous hydroxide, control ph 3.0-4.0, blasts atmospheric oxidation and obtain iron oxide seed crystal in solution, 2Fe (OH)
2+ 1/2O
2→ Fe
2o
3h
2o+H
2o;
6. will obtain iron oxide seed crystal solution drops in oxidation tank, iron sheet and/or iron powder is added to the iron oxide seed crystal solution in oxidation tank, quantitatively copperas solution is added in solution, steam heating solution is passed in the solution in oxidation tank, and pass into atmospheric oxidation ferrous ion and obtain iron ion, the hydroxide radical of iron ion in water is combined and is deposited on iron oxide seed crystal on the surface, form iron oxide yellow gradually, the hydrogen ion produced while oxidizing reaction and iron sheet and/or iron powder react, generate ferrous ion and be oxidized to iron ion again, until oxidizing reaction terminates;
7. obtained iron oxide yellow solution is entered in pressure filter, carry out solid-liquid separation, obtain mother liquid coming and filter residue, press filtration again after the filter residue washing obtained after solid-liquid separation, drying operation is carried out after obtaining clean filter residue, after filter residue after oven dry is pulverized, obtain finished product iron oxide yellow powder packaging warehouse-in.
Step 2. in reactive tank, pass into steam, make acid waste water be heated to 50-60 DEG C.
Step 2. in stop adding iron sheet and/or iron powder when sulfuric acid content is reduced to below 10% in reactive tank.
Step 2. in when passing into steam in reactive tank, with water vapor volatilization sulfuric acid mist waste gas carry out centralized collection after enter alkali lye spray absorber.
Step 5. described in alkali lye be sodium hydroxide solution, occur FeSO
4+ 2NaOH → Fe (OH)
2+ Na
2sO
4reaction.
In described sodium hydroxide solution, the mass percent of sodium hydroxide is 30%.
5. step carries out at the temperature of 20-30 DEG C.
Step keeps solution temperature 80-85 DEG C when 6. passing into steam.
Step 6. time keep the pH value of solution between 3.0-4.0.
The invention has the beneficial effects as follows, the method of titanium dioxide industry acid waste water production iron oxide yellow of the present invention achieves the nuisanceless disposal of the acid waste water that titanium dioxide industry is produced, resource utilization is recycled, and obtains calcium sulphate powders and iron oxide yellow powder, can be used for other industrial raw material.
Embodiment
A kind of titanium dioxide industry acid waste water of the present invention produces the method for iron oxide yellow, has following steps:
1. the raw material acid waste water containing ferrous sulfate and sulfuric acid is entered reactive tank;
2. in reactive tank, add iron sheet and/or iron powder, in reactive tank, pass into steam, acid waste water is heated, promote that iron sheet and/or iron powder and sulfuric acid carry out Fe+H
2sO
4→ FeSO
4+ H
2↑ reaction, produces more ferrous sulfate;
3. after question response for some time, in reactive tank, add lime powder, and CaO+H is carried out in stirring
2sO
4→ CaSO
4+ H
2o neutralization reaction, make the remaining sulfuric acid in acid waste water generate calcium sulfate precipitation thing, the pH value to reactive tank inner acidic waste water reaches 3-4 and namely stops adding lime powder;
4. after reaction being completed, solution enters pressure filter and carries out press filtration, obtain ferrous sulfate waste water and calcium sulfate waste residues after press filtration, the ferrous sulfate waste water after press filtration is entered purification tank for liquid waste, the calcium sulfate waste residues after press filtration enters oven for drying, waste residue after drying is pulverized, makes calcium sulphate powders;
5. the ferrous sulfate waste water in purification tank for liquid waste is entered iron oxide seed crystal tank, in iron oxide seed crystal tank, metering adds alkali lye, and generate ferrous hydroxide, control ph 3.0-4.0, blasts atmospheric oxidation and obtain iron oxide seed crystal in solution, 2Fe (OH)
2+ 1/2O
2→ Fe
2o
3h
2o+H
2o;
6. will obtain iron oxide seed crystal solution drops in oxidation tank, iron sheet and/or iron powder is added to the iron oxide seed crystal solution in oxidation tank, quantitatively copperas solution is added in solution, steam heating solution is passed in the solution in oxidation tank, and pass into atmospheric oxidation ferrous ion and obtain iron ion, the hydroxide radical of iron ion in water is combined and is deposited on iron oxide seed crystal on the surface, form iron oxide yellow gradually, the hydrogen ion produced while oxidizing reaction and iron sheet and/or iron powder react, generate ferrous ion and be oxidized to iron ion again, until oxidizing reaction terminates;
7. obtained iron oxide yellow solution is entered in pressure filter, carry out solid-liquid separation, obtain mother liquid coming and filter residue, press filtration again after the filter residue washing obtained after solid-liquid separation, drying operation is carried out after obtaining clean filter residue, after filter residue after oven dry is pulverized, obtain finished product iron oxide yellow powder packaging warehouse-in.
Step 2. in reactive tank, pass into steam, make acid waste water be heated to 50-60 DEG C.Step 2. in stop adding iron sheet and/or iron powder when sulfuric acid content is reduced to below 10% in reactive tank.Step 2. in when passing into steam in reactive tank, with water vapor volatilization sulfuric acid mist waste gas carry out centralized collection after enter alkali lye spray absorber.
Step 5. described in alkali lye be sodium hydroxide solution, occur FeSO
4+ 2NaOH → Fe (OH)
2+ Na
2sO
4reaction.In described sodium hydroxide solution, the mass percent of sodium hydroxide is 30%.5. step carries out at the temperature of 20-30 DEG C.
Step keeps solution temperature 80-85 DEG C when 6. passing into steam.Step 6. time keep the pH value of solution between 3.0-4.0.
With above-mentioned according to desirable embodiment of the present invention for enlightenment, by above-mentioned description, relevant staff in the scope not departing from this invention technological thought, can carry out various change and amendment completely.The technical scope of this invention is not limited to the content on specification sheets, must determine its technical scope according to right.
Claims (9)
1. titanium dioxide industry acid waste water produces a method for iron oxide yellow, it is characterized in that having following steps:
1. the raw material acid waste water containing ferrous sulfate and sulfuric acid is entered reactive tank;
2. in reactive tank, add iron sheet and/or iron powder, in reactive tank, pass into steam, acid waste water is heated, promote that iron sheet and/or iron powder and sulfuric acid carry out Fe+H
2sO
4→ FeSO
4+ H
2↑ reaction, produces more ferrous sulfate;
3. after question response for some time, in reactive tank, add lime powder, and CaO+H is carried out in stirring
2sO
4→ CaSO
4+ H
2o neutralization reaction, make the remaining sulfuric acid in acid waste water generate calcium sulfate precipitation thing, the pH value to reactive tank inner acidic waste water reaches 3-4 and namely stops adding lime powder;
4. after reaction being completed, solution enters pressure filter and carries out press filtration, obtain ferrous sulfate waste water and calcium sulfate waste residues after press filtration, the ferrous sulfate waste water after press filtration is entered purification tank for liquid waste, the calcium sulfate waste residues after press filtration enters oven for drying, waste residue after drying is pulverized, makes calcium sulphate powders;
5. the ferrous sulfate waste water in purification tank for liquid waste is entered iron oxide seed crystal tank, in iron oxide seed crystal tank, metering adds alkali lye, and generate ferrous hydroxide, control ph 3.0-4.0, blasts atmospheric oxidation and obtain iron oxide seed crystal in solution, 2Fe (OH)
2+ 1/2O
2→ Fe
2o
3h
2o+H
2o;
6. will obtain iron oxide seed crystal solution drops in oxidation tank, iron sheet and/or iron powder is added to the iron oxide seed crystal solution in oxidation tank, quantitatively copperas solution is added in solution, steam heating solution is passed in the solution in oxidation tank, and pass into atmospheric oxidation ferrous ion and obtain iron ion, the hydroxide radical of iron ion in water is combined and is deposited on iron oxide seed crystal on the surface, form iron oxide yellow gradually, the hydrogen ion produced while oxidizing reaction and iron sheet and/or iron powder react, generate ferrous ion and be oxidized to iron ion again, until oxidizing reaction terminates;
7. obtained iron oxide yellow solution is entered in pressure filter, carry out solid-liquid separation, obtain mother liquid coming and filter residue, press filtration again after the filter residue washing obtained after solid-liquid separation, drying operation is carried out after obtaining clean filter residue, after filter residue after oven dry is pulverized, obtain finished product iron oxide yellow powder packaging warehouse-in.
2. titanium dioxide industry acid waste water as claimed in claim 1 produces the method for iron oxide yellow, it is characterized in that:
Step 2. in reactive tank, pass into steam, make acid waste water be heated to 50-60 DEG C.
3. titanium dioxide industry acid waste water as claimed in claim 1 or 2 produces the method for iron oxide yellow, it is characterized in that: step 2. in stop adding iron sheet and/or iron powder when sulfuric acid content is reduced to below 10% in reactive tank.
4. titanium dioxide industry acid waste water as claimed in claim 1 produces the method for iron oxide yellow, it is characterized in that: step 2. in when passing into steam in reactive tank, enter alkali lye spray absorber after carrying out centralized collection with the sulfuric acid mist waste gas of water vapor volatilization.
5. titanium dioxide industry acid waste water as claimed in claim 1 produces the method for iron oxide yellow, it is characterized in that: step 5. described in alkali lye be sodium hydroxide solution, there is FeSO
4+ 2NaOH → Fe (OH)
2+ Na
2sO
4reaction.
6. titanium dioxide industry acid waste water as claimed in claim 5 produces the method for iron oxide yellow, it is characterized in that: in described sodium hydroxide solution, the mass percent of sodium hydroxide is 30%.
7. titanium dioxide industry acid waste water as claimed in claim 5 produces the method for iron oxide yellow, it is characterized in that: 5. step carries out at the temperature of 20-30 DEG C.
8. titanium dioxide industry acid waste water as claimed in claim 1 produces the method for iron oxide yellow, it is characterized in that: keep solution temperature 80-85 DEG C when 6. step passes into steam.
9. titanium dioxide industry acid waste water as claimed in claim 8 produces the method for iron oxide yellow, it is characterized in that: step 6. time keep the pH value of solution between 3.0-4.0.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410666586.5A CN104478001A (en) | 2014-11-20 | 2014-11-20 | Method for producing iron oxide yellow from acidic waste water in titanium dioxide industry |
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|---|---|---|---|
| CN201410666586.5A CN104478001A (en) | 2014-11-20 | 2014-11-20 | Method for producing iron oxide yellow from acidic waste water in titanium dioxide industry |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105502512A (en) * | 2016-02-04 | 2016-04-20 | 天津大学 | Method for preparing iron oxide yellow from steel pickling wastewater |
| CN115895294A (en) * | 2022-11-22 | 2023-04-04 | 云浮鸿志新材料有限公司 | Composite nano transparent iron oxide yellow and preparation method thereof |
-
2014
- 2014-11-20 CN CN201410666586.5A patent/CN104478001A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105502512A (en) * | 2016-02-04 | 2016-04-20 | 天津大学 | Method for preparing iron oxide yellow from steel pickling wastewater |
| CN115895294A (en) * | 2022-11-22 | 2023-04-04 | 云浮鸿志新材料有限公司 | Composite nano transparent iron oxide yellow and preparation method thereof |
| CN115895294B (en) * | 2022-11-22 | 2023-10-03 | 云浮鸿志新材料有限公司 | Composite nano transparent iron oxide yellow and preparation method thereof |
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Application publication date: 20150401 |
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