CN107585791A - A kind of preparation method of iron oxide - Google Patents
A kind of preparation method of iron oxide Download PDFInfo
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- CN107585791A CN107585791A CN201710898902.5A CN201710898902A CN107585791A CN 107585791 A CN107585791 A CN 107585791A CN 201710898902 A CN201710898902 A CN 201710898902A CN 107585791 A CN107585791 A CN 107585791A
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Abstract
The invention discloses a kind of preparation method of iron oxide, comprise the following steps：(1) iron and steel pickling waste liquid is taken, iron powder is added, stirs, time of repose 24h；(2) stir and heat up, adjust the pH of pretreated iron and steel pickling waste liquid, add auxiliary agent, make final concentration of 50 65mg/l, stand filtering, obtain solution, survey Fe in solution2+Concentration；(3) the Part I solution for taking step (2) to obtain, being diluted with water makes Fe2+, agitator is stirred, is passed through air oxidation, obtains the liquid containing iron oxide seed crystal；(4) under agitation, water is added to make Fe Part II solution2+Concentration obtain the first solution for 0.2 0.8mol/l, the first solution is added in the liquid containing iron oxide seed crystal to obtain the second solution, blowing air oxidation, iron oxide yellow is made；(5) it is iron oxide yellow is filtered, separation washing, dry, grind and iron oxide is made.Product purity of the present invention is preferable, and whole technics comparing is simple.
Description
Technical field
The present invention relates to chemical technology field, and in particular to a kind of preparation method of iron oxide.
Background technology
Iron oxide, also known as burn limonite, burnt umber, colcother, iron oxide red, rouge and powder, Venetian red (main component is iron oxide)
Deng.Chemical formula Fe2O3, strong acid, middle strong acid are soluble in, outward appearance is red-brown powder.Its red-brown powder is a kind of rudimentary pigment,
It is industrial to claim iron oxide, for painting, in the industry such as ink, rubber, catalyst can be made, glass, jewel, the polishing agent of metal,
It can be used as iron-smelting raw material.
Iron oxide is hexagonal crystal system, and molecular formula is α-Fe2O3, there is nontoxic, alkaline-resisting, heat-resisting, decomposition temperature 1560
DEG C, in light red brown, become grey black in strong row calcination, but shape of being clayed into power becomes red again.Iron oxide extensively should
For industries such as building materials, paint, coating, papermaking, rubber, ceramics, glass and ink.Preparing the method for iron oxide has dry method and wet
Two kinds of method.Dry method is also known as green vitriol method, is to be dehydrated green vitriol in the equipment such as rotary kiln, tunnel cave, and oxidizing roasting removes SO42-, it is raw
Into iron oxide.A large amount of dust can be produced in the calcination process of dry process iron oxide, environmental pollution is larger；In addition, dry method system
Standby iron oxide product is second-rate.Wet method is also known as the precipitation method, makees raw material with green vitriol or ferric trichloride, adds alkali to be neutralized, profit
Fe (OH) is obtained with seeded crystallization, oxidation, precipitation3, it is calcined and obtains iron oxide.Wet method is prepared during iron oxide without SO2Waste gas is dirty
Dye, product quality are high.
Iron oxide is the main component of iron rust.The main reason of iron rust be ferrous metal in the presence of carbon impurity, with environment
In moisture and oxygen reaction, ferrous metal will get rusty.For painting, in the industry such as ink, rubber, catalyst can be made, glass,
The polishing agent of jewel, metal, can be used as iron-smelting raw material.Iron oxide maximum application is used as pigment.It is divided into by color
Iron oxide, iron oxide yellow, iron oxide black, iron oxide brown are mixed by iron oxide, iron oxide black (and iron oxide yellow)；Iron oxide
Orange is mixed by iron oxide and iron oxide yellow；Iron oxide green is mixed by the pthalocyanine blue and iron oxide yellow of blueness.
At present, a kind of preparation method of the preferable iron oxide of product purity is lacked.
The content of the invention
It is an object of the invention to provide a kind of preparation method of the preferable iron oxide of product purity.
To reach above-mentioned purpose, present invention employs following technical proposal：A kind of preparation method of iron oxide of the present invention,
Comprise the following steps：
(1) take iron and steel pickling waste liquid, add iron powder reducing ferric iron, make ferric mass percent account for total content to be
0.5-0.9%, stir, time of repose 24h；
(2) under agitation, stir and be warming up to 80-90 DEG C, pretreated iron and steel pickling waste liquid is adjusted with sodium acid carbonate
PH be 5-7, add auxiliary agent poly-iron chloride, make final concentration of 50-65mg/l, temperature is 50-70 DEG C, reaction time 1-2h,
Filtering is stood, the solution after double purification processing is obtained, surveys Fe in solution2+Concentration；Solution after double purification is handled is divided into
A part of solution and Part II solution；
(3) the Part I solution for taking step (2) to obtain, being diluted with water makes Fe2+For 0.2-0.8mol/l, regulation pH is 6-
8, temperature is 10-35 DEG C, and agitator is stirred, is passed through air oxidation, the pH for being oxidizing to solution is 4-5, must contain iron oxide yellow
The liquid of crystal seed；
(4) under agitation, water is added to make Fe Part II solution2+Concentration obtain the first solution for 0.2-0.8mol/l, will
First solution, which is added in the liquid containing iron oxide seed crystal, obtains the second solution, makes Fe in the liquid containing iron oxide seed crystal2+Molal quantity
Account for Fe in the second solution2+The 20-40% of molal quantity, regulation temperature are 70-90 DEG C, under the conditions of pH is 3.0-3.5, blowing air oxygen
Change, oxidization time 8-15h, iron oxide yellow is made；
(5) by filtering of the iron oxide yellow through coarse filter in step (4), after filter liquor is heated, then through fine filter again
Filtering and impurity removing is carried out, separation washing, through microwave dryer heat drying, grinds and iron oxide is made.
Further, in step (2), the volume ratio of the Part I solution and Part II solution is 2-2.5：8-
7.5。
Further, in step (3), the flow of the air is 0.1-0.2m3/h。
Further, in step (4), the flow of the air is 0.05-0.1m3/h。
Further, in step (3), the stir speed (S.S.) of the agitator is 500-800rpm.
Further, in step (5), the drying time is 2-3 hours.
Beneficial effect：Product purity of the present invention is preferable, and whole technics comparing is simple, pollutes small in production process, is produced into
This is low, and the performance of product is good, stable and controllable for quality.
Compared with prior art, the invention has the advantages that：
(1) present invention is handled iron and steel pickling waste liquid using a kind of easy impurity removal process, has obtained clear
The low iron content acid solution of impurity content, and using the acid solution after removal of impurities as raw material, versatile iron oxide yellow has been made, has realized
The recycling of steel acid pickle, turns waste into wealth.
(2) the final secondary caused solid, liquid, gas emission of the present invention reaches the discharge standard of national regulation.Realize zero
Discharge, is real clean preparation method.
Embodiment
The present invention is further described by following examples, but should be noted that the scope of the present invention is not implemented by these
Any restrictions of example.
Embodiment 1
The invention provides a kind of preparation method of iron oxide, comprise the following steps：
(1) take iron and steel pickling waste liquid, add iron powder reducing ferric iron, make ferric mass percent account for total content to be
0.5%, stir, time of repose 24h；
(2) under agitation, stir and be warming up to 85 DEG C, with the pH of the pretreated iron and steel pickling waste liquid of sodium acid carbonate regulation
For 6, auxiliary agent poly-iron chloride is added, makes final concentration of 50mg/l, temperature is 60 DEG C, reaction time 2h, stands filtering, obtains secondary
Solution after purified treatment, survey Fe in solution2+Concentration；Solution after double purification is handled is divided into Part I solution and second
Part solution；The volume ratio of the Part I solution and Part II solution is 2：7.5.
(3) the Part I solution for taking step (2) to obtain, being diluted with water makes Fe2+For 0.2mol/l, regulation pH is 6, temperature
For 25 DEG C, agitator is stirred, is passed through air oxidation, the pH for being oxidizing to solution is 4, obtains the liquid containing iron oxide seed crystal；
The flow of the air is 0.15m3/h；The stir speed (S.S.) of the agitator is 500rpm.
(4) under agitation, water is added to make Fe Part II solution2+Concentration obtain the first solution for 0.5mol/l, by first
Solution, which is added in the liquid containing iron oxide seed crystal, obtains the second solution, makes Fe in the liquid containing iron oxide seed crystal2+Molal quantity accounts for
Fe in two solution2+The 20% of molal quantity, regulation temperature are 80 DEG C, and under the conditions of pH is 3.0, blowing air aoxidizes, and oxidization time is
11h, iron oxide yellow is made；The flow of the air is 0.05/h.
(5) by filtering of the iron oxide yellow through coarse filter in step (4), after filter liquor is heated, then through fine filter again
Filtering and impurity removing is carried out, separation washing, through microwave dryer heat drying, grinds and iron oxide is made；The drying time is 2 small
When.
Embodiment 2
The difference of embodiment 2 and embodiment 1 is：The invention provides a kind of preparation method of iron oxide, including it is as follows
Step：
In step (1), iron and steel pickling waste liquid is taken, iron powder reducing ferric iron is added, accounts for ferric mass percent
Total content is 0.7%, is stirred, time of repose 24h；
In step (2), under agitation, stir and be warming up to 90 DEG C, pretreated steel acid is adjusted with sodium acid carbonate
The pH for washing waste liquid is 5, adds auxiliary agent poly-iron chloride, makes final concentration of 65mg/l, temperature is 50 DEG C, reaction time 1.5h, quiet
Filtering is put, the solution after double purification processing is obtained, surveys Fe in solution2+Concentration；Solution after double purification is handled is divided into first
Part solution and Part II solution；The volume ratio of the Part I solution and Part II solution is 2.3：7.
In step (3), the Part I solution of step (2) acquisition is taken, being diluted with water makes Fe2+For 0.5mol/l, regulation
PH is 8, and temperature is 35 DEG C, and agitator is stirred, is passed through air oxidation, and the pH for being oxidizing to solution is 4.5, must contain iron oxide yellow
The liquid of crystal seed；The flow of the air is 0.1m3/h；The stir speed (S.S.) of the agitator is 800rpm.
In step (4), under agitation, water is added to make Fe Part II solution2+Concentration for 0.8mol/l, to obtain first molten
Liquid, the first solution is added in the liquid containing iron oxide seed crystal and obtains the second solution, makes Fe in the liquid containing iron oxide seed crystal2+Rub
You account for Fe in the second solution by number2+The 40% of molal quantity, regulation temperature are 70 DEG C, under the conditions of pH is 3.5, blowing air oxidation, and oxygen
The change time is 8h, and iron oxide yellow is made；The flow of the air is 0.1m3/h。
In step (5), by filtering of the iron oxide yellow through coarse filter in step (4), after filter liquor is heated, then through smart mistake
Filter carries out filtering and impurity removing again, separation washing, through microwave dryer heat drying, grinds and iron oxide is made；When described dry
Between be 3 hours.
Embodiment 3
The difference of embodiment 3 and embodiment 1 is：The invention provides a kind of preparation method of iron oxide, including it is as follows
Step：
In step (1), iron and steel pickling waste liquid is taken, iron powder reducing ferric iron is added, accounts for ferric mass percent
Total content is 0.9%, is stirred, time of repose 24h；
In step (2), under agitation, stir and be warming up to 80- DEG C, pretreated steel acid is adjusted with sodium acid carbonate
The pH for washing waste liquid is 7, adds auxiliary agent poly-iron chloride, makes final concentration of 60mg/l, and temperature is 70 DEG C, reaction time 1h, is stood
Filtering, the solution after double purification processing is obtained, surveys Fe in solution2+Concentration；Solution after double purification is handled is divided into first
Divide solution and Part II solution；The volume ratio of the Part I solution and Part II solution is 2.5：8.
In step (3), the Part I solution of step (2) acquisition is taken, being diluted with water makes Fe2+For 0.8mol/l, regulation
PH is 7, and temperature is 10 DEG C, and agitator is stirred, is passed through air oxidation, and the pH for being oxidizing to solution is 5, is obtained brilliant containing iron oxide yellow
The liquid of kind；The flow of the air is 0.2m3/h；The stir speed (S.S.) of the agitator is 650rpm.
In step (4), under agitation, water is added to make Fe Part II solution2+Concentration for 0.2mol/l, to obtain first molten
Liquid, the first solution is added in the liquid containing iron oxide seed crystal and obtains the second solution, makes Fe in the liquid containing iron oxide seed crystal2+Rub
You account for Fe in the second solution by number2+The 30% of molal quantity, regulation temperature are 90 DEG C, under the conditions of pH is 3.25, blowing air oxidation, and oxygen
The change time is 15h, and iron oxide yellow is made；The flow of the air is 0.075m3/h。
In step (5), by filtering of the iron oxide yellow through coarse filter in step (4), after filter liquor is heated, then through smart mistake
Filter carries out filtering and impurity removing again, separation washing, through microwave dryer heat drying, grinds and iron oxide is made；When described dry
Between be 2.5 hours.
Experiment 1
Influence of the Fe powder addition to reaction rate
As shown in figure 1, with the increase of iron powder addition in acid pickle, system Fe2+Concentration accordingly increases, Fe2+Concentration increases
Big then system is acid to be reduced, and pH value rises therewith, because HCl concentration is larger when starting, the increase of Fe powder addition, surface is lived
Property big Fe powder amount is also relative increases, increase the surface area that Fe powder contacts with HCl, the Fe of generation2+Increase, H2It is a large amount of to separate out,
System pH rises comparatively fast, so reaction rate increases, but (the pH ＞ when HCl (58g/L) is depleted to smaller concentration in acid pickle
3.2), the Fe of generation2+And H2Gradually decrease, system reaction rate and pH value change are more and more slower.
Experiment 2
Iron oxide obtained by embodiment 1 to embodiment 3 is tested, it is as shown in table 1 to obtain test result：
| Project | Iron oxide | Silica | Alundum (Al2O3) |
| Embodiment 1 | 98.99 | 0.01 | 0.03 |
| Embodiment 2 | 98.50 | 0.02 | 0.02 |
| Embodiment 3 | 98.59 | 0.02 | 0.01 |
As shown in table 1, product purity of the invention is high, and impurity is few.
General principle, principal character and the advantages of the present invention of the present invention has been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the simply explanation described in above-described embodiment and specification is originally
The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, the present invention
Claimed scope is by appended claims, specification and its equivalent thereof.
Claims (6)
1. a kind of preparation method of iron oxide, it is characterised in that comprise the following steps：
(1) iron and steel pickling waste liquid is taken, adds iron powder reducing ferric iron, it is 0.5- ferric mass percent is accounted for total content
0.9%, stir, time of repose 24h；
(2) under agitation, stir and be warming up to 80-90 DEG C, with the pH of the pretreated iron and steel pickling waste liquid of sodium acid carbonate regulation
For 5-7, auxiliary agent poly-iron chloride is added, makes final concentration of 50-65mg/l, temperature is 50-70 DEG C, reaction time 1-2h, is stood
Filtering, the solution after double purification processing is obtained, surveys Fe in solution2+Concentration；
Solution after double purification is handled is divided into Part I solution and Part II solution；
(3) the Part I solution for taking step (2) to obtain, being diluted with water makes Fe2+For 0.2-0.8mol/l, regulation pH is 6-8, temperature
Spend for 10-35 DEG C, agitator is stirred, be passed through air oxidation, the pH for being oxidizing to solution is 4-5, must contain iron oxide seed crystal
Liquid；
(4) under agitation, water is added to make Fe Part II solution2+Concentration obtain the first solution for 0.2-0.8mol/l, by first
Solution, which is added in the liquid containing iron oxide seed crystal, obtains the second solution, makes Fe in the liquid containing iron oxide seed crystal2+Molal quantity accounts for
Fe in two solution2+The 20-40% of molal quantity, regulation temperature are 70-90 DEG C, under the conditions of pH is 3.0-3.5, blowing air oxidation,
Oxidization time is 8-15h, and iron oxide yellow is made；
(5) by filtering of the iron oxide yellow through coarse filter in step (4), after filter liquor is heated, then carry out again through fine filter
Filtering and impurity removing, separation washing, through microwave dryer heat drying, grind and iron oxide is made.
2. the preparation method of iron oxide according to claim 1, it is characterised in that：In step (2), the Part I
The volume ratio of solution and Part II solution is 2-2.5：8-7.5.
3. the preparation method of iron oxide according to claim 1 or 2, it is characterised in that：In step (3), the air
Flow be 0.1-0.2m3/h。
4. the preparation method of iron oxide according to claim 3, it is characterised in that：In step (4), the stream of the air
Measure as 0.05-0.1m3/h。
5. the preparation method of iron oxide according to claim 1, it is characterised in that：In step (3), the agitator
Stir speed (S.S.) is 500-800rpm.
6. the preparation method of the iron oxide according to any one of claim 1 to 5, it is characterised in that：In step (5), institute
It is 2-3 hours to state drying time.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109384263A (en) * | 2018-11-08 | 2019-02-26 | 中国神华能源股份有限公司 | A method of iron oxide yellow is prepared using the waste acid liquor of chloride containing iron |
| CN110217826A (en) * | 2019-07-02 | 2019-09-10 | 浙江华源颜料股份有限公司 | A kind of preparation method of the low viscosity iron oxide yellow of microwave intervention |
Citations (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 |
| CN105753068A (en) * | 2016-02-04 | 2016-07-13 | 河北爱德斯蒂尔环保科技有限公司 | Method for preparing iron oxide red through steel acid pickling waste liquor |
-
2017
- 2017-09-28 CN CN201710898902.5A patent/CN107585791A/en active Pending
Patent Citations (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 |
| CN105753068A (en) * | 2016-02-04 | 2016-07-13 | 河北爱德斯蒂尔环保科技有限公司 | Method for preparing iron oxide red through steel acid pickling waste liquor |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109384263A (en) * | 2018-11-08 | 2019-02-26 | 中国神华能源股份有限公司 | A method of iron oxide yellow is prepared using the waste acid liquor of chloride containing iron |
| CN110217826A (en) * | 2019-07-02 | 2019-09-10 | 浙江华源颜料股份有限公司 | A kind of preparation method of the low viscosity iron oxide yellow of microwave intervention |
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