CN104402061A - Production process for preparing iron oxide black by ferrous sulfate solution - Google Patents
Production process for preparing iron oxide black by ferrous sulfate solution Download PDFInfo
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- CN104402061A CN104402061A CN201410670710.5A CN201410670710A CN104402061A CN 104402061 A CN104402061 A CN 104402061A CN 201410670710 A CN201410670710 A CN 201410670710A CN 104402061 A CN104402061 A CN 104402061A
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- solution
- iron oxide
- oxide black
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Abstract
The invention relates to a production process for preparing iron oxide black by a ferrous sulfate solution. The production process comprises the following steps: (1) discharging the ferrous sulfate solution into a reaction tank; (2) adding a sodium hydroxide solution into the reaction tank, regulating the pH value to alkalinity and generating a ferrous hydroxide solution; (3) introducing air and steam into the solution, carrying out heating oxidation reaction and gradually forming ferrous hydroxide and other intermediate transitional mixed floccules; (4) after heating oxidation reaction for a certain time, gradually dewatering and decomposing, and generating small particles of ferroferric oxide; (5) discharging a prepared ferroferric oxide solution into a filter press and carrying out solid-liquid separation to obtain mother liquid water and filter residues; (6) washing the obtained filter residues, then carrying out filter pressing and obtaining clear ferroferric oxide filter residues and drying by using a drying box; (7) crushing the dried filter residues, packaging and warehousing. According to the production process, recycling of the ferrous sulfate solution is realized, and the iron oxide black is obtained and can be used for preparing pigments.
Description
Technical field
The present invention relates to iron oxide black technical field of producing, especially a kind of copperas solution prepares the production technique of iron oxide black.
Background technology
Z 250, chemical formula Fe
3o
4, another name iron oxide black, the production method of domestic and international iron oxide black has usually: three classes such as pure iron oxidizing combustion method, iron powder reducing method, mixed molysite (ferrous and trivalent iron salt) conversion method.
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 make iron oxide black, and iron oxide black can be used for preparing pigment.
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 black, and it is simple that copperas solution prepares iron oxide black technique, and no coupling product, non-exhaust emission.
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 black, has following steps:
1. copperas solution is entered retort;
2. in retort, add the sodium hydroxide solution of massfraction 30%, adjust ph is to 8-9, FeSO
4+ 2NaOH → Fe (OH)
2+ Na
2sO
4generate hydroxide ferrous solution;
3. add to solution and pass into air and high-temperature steam, carry out heating oxidizing reaction, 4Fe (OH)
2+ O
2+ 2H
2o → 4Fe (OH)
3form ferrous hydroxide and other middle transition mixing floss gradually;
4. after oxidizing reaction certain hour of heating, kinetics Fe (OH) gradually
2+ 2Fe (OH)
3→ Fe
3o
4+ 4H
2o, generates short grained Z 250;
5. the Z 250 solution of above-mentioned preparation is entered in pressure filter, carry out solid-liquid separation, obtain mother liquid coming and filter residue;
6. the filter residue obtained is washed, again carry out press filtration, obtain clean Z 250 filter residue by oven for drying, airtight chain-arranged type baking oven can be adopted to carry out drying with steam;
7., after the filter residue after oven dry being pulverized, obtain finished product iron oxide black powder packaging warehouse-in, high speed centrifugation pulverizer can be adopted to pulverize.
Step 2. in sodium hydroxide solution the massfraction of sodium hydroxide be 30%.
Further, step 2. in solution is adjusted to pH value is 9 ± 0.5.
Further, step 3. in control solution temperature be 80 ± 5 DEG C.
Further, step 4. in oxidation time of heating be 3-4 hour.
The invention has the beneficial effects as follows, the production technique that copperas solution of the present invention prepares iron oxide black achieves the recycling of copperas solution, obtains iron oxide black, can be used for pigment preparation, the comprehensive resource process of real waste water.
Embodiment
Copperas solution of the present invention prepares the production technique of iron oxide black, has following steps:
1. copperas solution is entered retort;
2. in retort, add the sodium hydroxide solution of massfraction 30%, adjust ph is to 8-9, FeSO
4+ 2NaOH → Fe (OH)
2+ Na
2sO
4generate hydroxide ferrous solution;
3. add to solution and pass into air and steam, carry out heating oxidizing reaction, 4Fe (OH)
2+ O
2+ 2H
2o → 4Fe (OH)
3form ferrous hydroxide and other middle transition mixing floss gradually;
4. after oxidizing reaction certain hour of heating, kinetics Fe (OH) gradually
2+ 2Fe (OH)
3→ Fe
3o
4+ 4H
2o, generates short grained Z 250;
5. the Z 250 solution of above-mentioned preparation is entered in pressure filter, carry out solid-liquid separation, obtain mother liquid coming and filter residue;
6. the filter residue obtained is washed, again carry out press filtration, obtain clean Z 250 filter residue and pass through oven for drying;
7., after being pulverized by the filter residue after oven dry, finished product iron oxide black powder packaging warehouse-in is obtained.
Step 2. in sodium hydroxide solution the massfraction of sodium hydroxide be 30%.
Further, step 2. in solution is adjusted to pH value is 9 ± 0.5.
Further, step 3. in control solution temperature be 80 ± 5 DEG C.
Further, step 4. in oxidation time of heating be 3-4 hour.
Step 5. in the mother liquid coming that obtains can also be used in the production of construction materials processes such as flyash standard brick spice water, realize comprehensive utilization.
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 (5)
1. copperas solution prepares a production technique for iron oxide black, it is characterized in that having following steps:
1. copperas solution is entered retort;
2. in retort, add sodium hydroxide solution, adjust ph is to 8-9, FeSO
4+ 2NaOH → Fe (OH)
2+ Na
2sO
4generate hydroxide ferrous solution;
3. add to solution and pass into air and steam, carry out heating oxidizing reaction, 4Fe (OH)
2+ O
2+ 2H
2o → 4Fe (OH)
3form ferrous hydroxide and other middle transition mixing floss gradually;
4. after oxidizing reaction certain hour of heating, kinetics Fe (OH) gradually
2+ 2Fe (OH)
3→ Fe
3o
4+ 4H
2o, generates short grained Z 250;
5. the Z 250 solution of above-mentioned preparation is entered in pressure filter, carry out solid-liquid separation, obtain mother liquid coming and filter residue;
6. the filter residue obtained is washed, again carry out press filtration, obtain clean Z 250 filter residue and pass through oven for drying;
7., after being pulverized by the filter residue after oven dry, finished product iron oxide black powder packaging warehouse-in is obtained.
2. copperas solution as claimed in claim 1 prepares the production technique of iron oxide black, it is characterized in that: step 2. in sodium hydroxide solution the massfraction of sodium hydroxide be 30%.
3. copperas solution as claimed in claim 1 prepares the production technique of iron oxide black, it is characterized in that: step 2. in solution is adjusted to pH value is 9 ± 0.5.
4. copperas solution as claimed in claim 1 prepares the production technique of iron oxide black, it is characterized in that: step 3. middle control solution temperature is 80 ± 5 DEG C.
5. copperas solution as claimed in claim 1 prepares the production technique of iron oxide black, it is characterized in that: step 4. in oxidation time of heating be 3-4 hour.
Priority Applications (1)
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CN201410670710.5A CN104402061A (en) | 2014-11-21 | 2014-11-21 | Production process for preparing iron oxide black by ferrous sulfate solution |
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CN201410670710.5A CN104402061A (en) | 2014-11-21 | 2014-11-21 | Production process for preparing iron oxide black by ferrous sulfate solution |
Publications (1)
Publication Number | Publication Date |
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CN104402061A true CN104402061A (en) | 2015-03-11 |
Family
ID=52639748
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107200362A (en) * | 2017-06-26 | 2017-09-26 | 杭州明兴化工有限公司 | A kind of method that pure oxygen oxidizing process produces iron oxide black |
CN110316765A (en) * | 2019-07-02 | 2019-10-11 | 浙江华源颜料股份有限公司 | A kind of preparation method of low viscosity black iron oxide pigment |
-
2014
- 2014-11-21 CN CN201410670710.5A patent/CN104402061A/en active Pending
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107200362A (en) * | 2017-06-26 | 2017-09-26 | 杭州明兴化工有限公司 | A kind of method that pure oxygen oxidizing process produces iron oxide black |
CN110316765A (en) * | 2019-07-02 | 2019-10-11 | 浙江华源颜料股份有限公司 | A kind of preparation method of low viscosity black iron oxide pigment |
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PB01 | Publication | ||
WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150311 |
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