CN104445433A - Production process for preparing iron oxide yellow by using ferrous sulfate solution - Google Patents

Production process for preparing iron oxide yellow by using ferrous sulfate solution Download PDF

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Publication number
CN104445433A
CN104445433A CN201410670526.0A CN201410670526A CN104445433A CN 104445433 A CN104445433 A CN 104445433A CN 201410670526 A CN201410670526 A CN 201410670526A CN 104445433 A CN104445433 A CN 104445433A
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solution
iron oxide
iron
oxide yellow
seed crystal
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CN201410670526.0A
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周淑华
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Abstract

The invention discloses a production process for preparing iron oxide yellow by using a ferrous sulfate solution. The production process comprises the following steps: (1) discharging the ferrous sulfate solution into an iron oxide yellow seed crystal tank; (2) adding measured alkali liquor into the iron oxide yellow seed crystal tank to generate ferrous hydroxide, and controlling the pH value between 3.0 and 4.0; (3) blowing air into the solution to realize oxidation to prepare an iron oxide yellow seed crystal; (4) putting the prepared iron oxide yellow seed crystal solution into an oxidation tank; (5) adding iron sheets and/or iron dust into the iron oxide yellow seed crystal solution in the oxidation tank; (6) quantitatively adding a ferrous sulfate solution into the solution; and (7) introducing steam into the solution in the oxidation tank to heat the solution, and introducing air to oxidize ferrous ions to obtain iron ions, wherein the iron ions are combined with hydroxy radicals in water and are deposited on the surface of the iron oxide yellow seed crystal to gradually form iron oxide yellow, and the hydrogen ions generated during an oxidation reaction react with the iron sheets and/or iron dust to generate ferrous ions which are oxidized into iron ions until the oxidation reaction is finished. By adopting the production process disclosed by the invention, the recycling of the ferrous sulfate solution is realized.

Description

Copperas solution prepares the production technique of iron oxide yellow
Technical field
The present invention relates to the production technique of iron oxide yellow, especially a kind of copperas solution prepares the production technique of 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 copperas solution to prepare the production technique of iron oxide yellow, achieve ferrous sulfate waste water and prepare iron protoxide, realize recycling.
The technical solution adopted for the present invention to solve the technical problems is: a kind of copperas solution prepares the production technique of iron oxide yellow, has following steps:
1. copperas solution is entered iron oxide seed crystal tank;
2. in iron oxide seed crystal tank, metering adds alkali lye, generates ferrous hydroxide, control ph 3.0-4.0;
3. in solution, blast atmospheric oxidation and obtain iron oxide seed crystal, 2Fe (OH) 2+ 1/2O 2→ Fe 2o 3h 2o+H 2o;
4. drop in oxidation tank to obtained iron oxide seed crystal solution;
5. iron sheet and/or iron powder is added to the iron oxide seed crystal solution in oxidation tank;
6. in solution, quantitatively copperas solution is added;
7. in the solution in oxidation tank, pass into steam heating solution, and pass into atmospheric oxidation ferrous ion (Fe 2+) obtain iron ion (Fe 3+), the hydroxide radical of iron ion in water is combined and is deposited on iron oxide seed crystal on the surface, forms iron oxide yellow gradually, and 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;
8. obtained iron oxide yellow solution is entered in pressure filter, carry out solid-liquid separation, obtain mother liquid coming and filter residue;
9. press filtration again after the filter residue washing obtained after solid-liquid separation, carries out drying operation after obtaining clean filter residue;
10., after the filter residue after oven dry being pulverized, finished product iron oxide yellow powder packaging warehouse-in is obtained.
As preferably, step 2. described in alkali lye be sodium hydroxide solution, there is FeSO 4+ 2NaOH → Fe (OH) 2+ Na 2sO 4reaction.
Further, in described sodium hydroxide solution, the mass percent of sodium hydroxide is 30%.
Further, 3. step carries out at the temperature of 20-30 DEG C.
Further, solution temperature 80-85 DEG C is kept when 7. step passes into steam.Suitable temperature can accelerate speed of reaction.
Further, step 7. time keep the pH value of solution between 3.0-4.0.
The invention has the beneficial effects as follows, the production technique that copperas solution of the present invention prepares iron oxide yellow achieves the recycling of copperas solution, obtains iron oxide yellow, can be used for pigment preparation, the comprehensive resource process of real waste water.
Embodiment
A kind of copperas solution of the present invention prepares the production technique of iron oxide yellow, has following steps:
1. copperas solution is entered iron oxide seed crystal tank;
2. in iron oxide seed crystal tank, metering adds alkali lye, generates ferrous hydroxide, control ph 3.0-4.0;
3. in solution, blast atmospheric oxidation and obtain iron oxide seed crystal, 2Fe (OH) 2+ 1/2O 2→ Fe 2o 3h 2o+H 2o;
4. drop in oxidation tank to obtained iron oxide seed crystal solution;
5. iron sheet and/or iron powder is added to the iron oxide seed crystal solution in oxidation tank;
6. in solution, quantitatively copperas solution is added;
7. in the solution in oxidation tank, pass into steam heating solution, and pass into atmospheric oxidation ferrous ion (Fe 2+) obtain iron ion (Fe 3+), iron ion (Fe 3+) hydroxide radical 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 react with iron sheet and/or iron powder, and generation ferrous ion is also oxidized to iron ion again, until oxidizing reaction terminates, and 2FeSO 47H 2o+1/2O 2+ 2H 2o → Fe 2o 3h 2o+2H 2sO 4+ 6H 2o, H 2sO 4+ Fe → FeSO 4+ H 2↑;
8. obtained iron oxide yellow solution is entered in pressure filter, carry out solid-liquid separation, obtain mother liquid coming and filter residue;
9. press filtration again after the filter residue washing obtained after solid-liquid separation, carries out drying operation after obtaining clean filter residue, adopts airtight chain-arranged type baking oven to carry out drying with steam;
10., after pulverizing the filter residue after oven dry, obtain finished product iron oxide yellow powder packaging warehouse-in, high speed centrifugation pulverizer is pulverized.
As preferably, step 2. described in alkali lye be sodium hydroxide solution, there is FeSO 4+ 2NaOH → Fe (OH) 2+ Na 2sO 4reaction.
Further, in described sodium hydroxide solution, the mass percent of sodium hydroxide is 30%.
Further, 3. step carries out at the temperature of 20-30 DEG C.
Further, solution temperature 80-85 DEG C is kept when 7. step passes into steam.Suitable temperature can accelerate speed of reaction.
Further, step 7. time keep the pH value of solution between 3.0-4.0.
Step 8. in the first mother liquid coming that obtains can enter pond for recovering and recycling in iron oxide black production technique; Step 9. in the second mother liquid coming that obtains directly enter purification tank for liquid waste and discharge behind neutralization precipitation pond.
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 (6)

1. copperas solution prepares a production technique for iron oxide yellow, it is characterized in that having following steps:
1. copperas solution is entered iron oxide seed crystal tank;
2. in iron oxide seed crystal tank, metering adds alkali lye, generates ferrous hydroxide, control ph 3.0-4.0;
3. in solution, blast atmospheric oxidation and obtain iron oxide seed crystal, 2Fe (OH) 2+ 1/2O 2→ Fe 2o 3h 2o+H 2o;
4. will obtain iron oxide seed crystal solution drops in oxidation tank;
5. iron sheet and/or iron powder is added to the iron oxide seed crystal solution in oxidation tank;
6. in solution, quantitatively copperas solution is added;
7. in the solution in oxidation tank, steam heating solution is passed into, 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;
8. obtained iron oxide yellow solution is entered in pressure filter, carry out solid-liquid separation, obtain mother liquid coming and filter residue;
9. press filtration again after the filter residue washing obtained after solid-liquid separation, carries out drying operation after obtaining clean filter residue;
10., after the filter residue after oven dry being pulverized, finished product iron oxide yellow powder packaging warehouse-in is obtained.
2. copperas solution as claimed in claim 1 prepares the production technique of iron oxide yellow, it is characterized in that: step 2. described in alkali lye be sodium hydroxide solution, there is FeSO 4+ 2NaOH → Fe (OH) 2+ Na 2sO 4reaction.
3. copperas solution as claimed in claim 2 prepares the production technique of iron oxide yellow, it is characterized in that: in described sodium hydroxide solution, the mass percent of sodium hydroxide is 30%.
4. copperas solution as claimed in claim 1 prepares the production technique of iron oxide yellow, it is characterized in that: 3. step carries out at the temperature of 20-30 DEG C.
5. copperas solution as claimed in claim 1 prepares the production technique of iron oxide yellow, it is characterized in that: keep solution temperature 80-85 DEG C when 7. step passes into steam.
6. copperas solution as claimed in claim 5 prepares the production technique of iron oxide yellow, it is characterized in that: step 7. time keep the pH value of solution between 3.0-4.0.
CN201410670526.0A 2014-11-21 2014-11-21 Production process for preparing iron oxide yellow by using ferrous sulfate solution Pending CN104445433A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106966434A (en) * 2017-03-25 2017-07-21 杭州明兴化工有限公司 A kind of method that hermetically sealed dioxygen oxidation method produces iron oxide
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

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106966434A (en) * 2017-03-25 2017-07-21 杭州明兴化工有限公司 A kind of method that hermetically sealed dioxygen oxidation method produces iron oxide
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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