CN101607741B - Method for preparing iron oxide red by byproduct ferrous sulfate of titanium dioxide - Google Patents
Method for preparing iron oxide red by byproduct ferrous sulfate of titanium dioxide Download PDFInfo
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Abstract
The invention discloses a method for preparing iron oxide red by taking byproduct ferrous sulfate of titanium dioxide as a raw material. The method comprises the following steps: purifying the byproduct ferrous sulfate, removing impurities, pouring the purified ferrous sulfate solution into a container, stirring the solution and adding ammonia water, adjusting the pH value of the solution to be between 6.5 and 9, and stopping the addition of ammonia water; washing and filtering the obtained material, and stopping until the pH value of the solution is between 6.5 and 7 to obtain filter cake and filtrate; and calcining the obtained filter cake in a rotary kiln to obtain an iron oxide red semi-finished product, putting the semi-finished product into a ball mill, adding water for ball milling, washing, filtering and drying the obtain material after ball milling, and crushing after drying to obtain an iron oxide red product. The method solves the problem of treating the byproduct for titanium dioxide manufacturers, is favorable for environmental protection, and reduces the production cost of iron oxide red; and the iron oxide red prepared by the method is mainly used in aspects of coloring agents, antirust paint pigment, ceramic pigment of building materials, polishing agents of precision parts, and the like.
Description
One, technical field:
The present invention relates to a kind of preparation method of red iron oxide, particularly relate to a kind of method of utilizing byproduct ferrous sulfate of titanium dioxide to prepare red iron oxide.
Two, background technology:
Red iron oxide is a kind of common mineral dye, is widely used in fields such as coating, building materials, plastics, electronics; High-purity red iron oxide can be used as the rumbling compound of opticglass, senior abrasive substance.The common production method of red iron oxide mainly contains following two kinds:
First kind is the green vitriol calcination method: this method is to be that raw material carries out high-temperature calcination with purified green vitriol, the red iron oxide of generation through washing, dry, be crushed into product.
Second kind is the wet method air oxidation process: the main raw material of this method is an iron sheet, production process is from the preparation crystal seed, adopt sulfuric acid or nitric acid to prepare crystal seed, crystal seed is added in the second oxidation bucket, add iron sheet and water, adding ferrous salt again is reaction medium, and steam is warmed up to more than 70 ℃, under certain pH value condition, blast atmospheric oxidation, obtain red iron oxide and iron oxide yellow.
The main raw material of the wet type method for producing of above-mentioned red iron oxide is iron sheet and sulfuric acid, and raw material route has limited the production of red iron oxide to a certain extent; Simultaneously, in the sulfuric acid method titanium pigment production process, produced a large amount of by-product ferrous sulfate durings, 1 ton of titanium dioxide of every production has 4 tons of ferrous sulfate of by product approximately, if and by-product ferrous sulfate during can not get rationally utilizing fully, not only can become the burden that sulfuric acid method titanium pigment is produced, but also can cause to a certain degree environmental pollution, do not utilize environmental protection.
About the handling problem of titanium dioxide ferrous sulfate as side product, just used it for as aspects such as iron catalyst, water purification agent, fodder additives, soil improvement agents, but the quantity of treatable titanium dioxide ferrous sulfate as side product seldom in the past.Can be effective and utilize the titanium dioxide ferrous sulfate as side product to prepare iron oxide pigment, on the one hand can the mass consumption ferrous sulfate as side product, iron oxide pigment per ton approximately can consume 4 tons of ferrous sulfate as side product, the performance of the iron oxide pigment of Sheng Chaning is also relatively good on the other hand, market outlet is good, and demand is big.At present, also have much about the bibliographical information that utilizes byproduct ferrous sulfate of titanium dioxide production red iron oxide and iron oxide yellow, for example: 1, application number is 03150766.2, denomination of invention is a kind of preparation method of ferric oxide red powder, this method is to be raw material with the byproduct ferrous sulfate that produces in the production process of titanium pigment, by purification and impurity removal, precipitation demanganize, processes such as washing and torch firing are produced high-purity soft magnetism ferric oxide red powder.2, application number is 02148428.7, denomination of invention is produced the method for ferric oxide red colorant for the titanium white ferrous sulfate as side product, it is raw material that this method discloses with the titanium dioxide ferrous sulfate as side product, earlier to ferrous sulfate make with extra care, prepare then crystal seed, oxidation synthetic, filter, washing, oven dry, pulverize last packaging final prod.
Three, summary of the invention:
It is the method for feedstock production red iron oxide with the byproduct ferrous sulfate of titanium dioxide that the technical problem to be solved in the present invention provides a kind of.
Address the above problem, the technical solution used in the present invention is:
The invention provides a kind of method of utilizing byproduct ferrous sulfate of titanium dioxide to prepare red iron oxide, described method is to be raw material with the by-product ferrous sulfate during that produces in the production process of titanium pigment, earlier with its purification and impurity removal, make further prepared in reaction with the copperas solution after purifying then and become the red iron oxide product, its detailed step is as follows:
The purification and impurity removal of a, ferrous sulfate: earlier byproduct ferrous sulfate of titanium dioxide is imported in the container of belt stirrer and stir, constantly add entry in the whipping process, it is fully dissolved, the degree Beaume of adjusting solution is 20～35, put into flocculation agent then, the add-on of flocculation agent is 0.1～0.8% of a ferrous sulfate gross weight, stirring, static more than 2 hours, and static back supernatant liquid is the copperas solution after purifying;
B, step a gained clear liquid copperas solution is extracted in the container of another belt stirrer and stirs, slowly add ammoniacal liquor in whipping process, the concentration of ammoniacal liquor is 15～20%, it is fully reacted, when the pH of solution value is 6.5～9, stop to add ammoniacal liquor, i.e. reaction stops;
C, step b gained material is washed, filters, treat that pH value of filtrate is to stop, and obtains filter cake and filtrate at 6.5～7 o'clock;
D, step c gained filter cake is calcined with kiln, continuous bubbling air in calcination process, calcining temperature is 700～1000 ℃, calcination time is 2～6 hours, obtains the work in-process red iron oxide after the calcining;
E, steps d gained work in-process red iron oxide is put into ball mill and added entry, the weight ratio that work in-process red iron oxide and water add is 1: 0.5～1, ball milling 1～2 hour, behind the ball milling gained material is washed, filtered and dries, bake out temperature is 180～200 ℃, drying time is 1～1.5 hour, is crushed to after the oven dry and promptly gets the red iron oxide product more than 320 orders.
For above-mentioned a kind of method of utilizing byproduct ferrous sulfate of titanium dioxide to prepare red iron oxide, the percentage composition of ferrous sulfate is 85～92% in the described byproduct ferrous sulfate of titanium dioxide.
For above-mentioned a kind of method of utilizing byproduct ferrous sulfate of titanium dioxide to prepare red iron oxide, the stirring velocity of agitator described in the step a is 30 rev/mins～42 rev/mins; Described flocculation agent is a polyacrylamide, and its molecular weight is 3,000,000, and consumption calculates by 100% polyacrylamide.
For above-mentioned a kind of method of utilizing byproduct ferrous sulfate of titanium dioxide to prepare red iron oxide, the container bottom residual precipitate of static back described in the step a enters in the useless vice processing pond of red iron oxide in producing, and focuses on qualified discharge.
For above-mentioned a kind of method of utilizing byproduct ferrous sulfate of titanium dioxide to prepare red iron oxide, the stirring velocity of agitator described in the step b is 30 rev/mins～42 rev/mins; The preferred range of described pH value is 6.5～7.5;
For above-mentioned a kind of method of utilizing byproduct ferrous sulfate of titanium dioxide to prepare red iron oxide, filtrate described in the step c is ammoniumsulphate soln, is that 18～22 o'clock direct composite fertilizer factories that supply with are as raw material with its evaporation concentration to degree Beaume.
For above-mentioned a kind of method of utilizing byproduct ferrous sulfate of titanium dioxide to prepare red iron oxide, kiln described in the steps d adopts rotary kiln, and the preferred range of described calcining temperature is 800～900 ℃.
For above-mentioned a kind of method of utilizing byproduct ferrous sulfate of titanium dioxide to prepare red iron oxide, the rotary kiln snead process is adopted in oven dry described in the step e; Described water lotion through washing returns step a and recycles.
Utilizing byproduct ferrous sulfate of titanium dioxide to prepare in the method for red iron oxide, plate filter is all adopted in described filtration.
Positive beneficial effect of the present invention:
1, to adopt the useless by-product ferrous sulfate during that produces in the production process of titanium pigment be the feedstock production red iron oxide in the present invention; not only solved the problem of handling byproduct for titanium white production producer; help environment protection, and reduced the production cost of red iron oxide.
2, production process of the present invention is simple, enforcement easy to operate, easy.
3, in the preparation method of red iron oxide of the present invention, gained filtrate is ammoniumsulphate soln among the step c, is that 18～22 o'clock direct composite fertilizer factories that supply with are as raw material with its evaporation concentration to degree Beaume; The gained washings returns among the step a and recycles among the step e, thereby, in production process of the present invention, there are not refuse, discharging of waste liquid, be difficult for causing environmental pollution, help environmental protection.
4, adopt the red iron oxide of the inventive method preparation, its purity can reach more than 95%, is mainly used in the aspects such as rumbling compound of tinting material, rust-inhibiting paint pigment, beramic color and the precision part of building materials.
Four, embodiment:
Following examples only in order to further specify the present invention, do not limit content of the present invention.
Raw material: ferrous sulfate is the by-product ferrous sulfate during that produces in the Titanium White Production By Sulfuric Acid Process process, and its percentage composition is 86～92%.
Embodiment one: a kind of method of utilizing byproduct ferrous sulfate of titanium dioxide to prepare red iron oxide
Its concrete steps are as follows:
A, the purification and impurity removal of ferrous sulfate: earlier 9 tons of byproduct ferrous sulfate of titanium dioxide are imported in the container of belt stirrer, the percentage composition of ferrous sulfate is 90%, starting agitator stirs, stirring velocity is 30 rev/mins～42 rev/mins, constantly add entry in the whipping process, it is fully dissolved, adjust the degree Beaume to 30 of solution, put into the flocculation agent polyacrylamide then, the add-on of polyacrylamide is 0.1% of a ferrous sulfate total amount, stirs, static 3 hours, static back gained supernatant liquid was the copperas solution after purifying, the container bottom residual precipitate enters in the useless vice processing pond of ferric oxide red colorant in producing, and focuses on qualified discharge;
B, step a gained clear liquid copperas solution is extracted in the container of another belt stirrer, starting agitator stirs, stirring velocity is 30 rev/mins～42 rev/mins, slow adding concentration is 15% ammoniacal liquor in whipping process, it is fully reacted, when the pH of solution value is 6.5, stop to add ammoniacal liquor, i.e. reaction stops;
C, step b gained material is washed, filters, treat that pH value of filtrate is to stop at 7 o'clock, obtain filter cake and filtrate, gained ammonium sulfate filtrate is concentrated, directly supply with composite fertilizer factory as raw material when degree Beaume is 20 when filtrate is concentrated to;
D, step c gained filter cake is calcined with rotary kiln, continuous bubbling air in calcination process, calcining temperature is 850 ℃, calcination time is 4 hours, obtains the work in-process red iron oxide after the calcining;
E, steps d gained work in-process are put into ball mill and added entry, the weight ratio that work in-process red iron oxide and water add is 1: 0.5, ball milling 1 hour, behind the ball milling gained material is washed, filtered, adopt the rotary kiln snead process to dry then, bake out temperature is 200 ℃, and drying time is 1 hour, after the oven dry it is crushed to and promptly gets the red iron oxide product more than 320 orders, through weighing 2.14 tons of gained red iron oxides.
Among the step e water lotion after the gained material washing returned among the step a and use as solvent cycle.
Embodiment two: a kind of method of utilizing byproduct ferrous sulfate of titanium dioxide to prepare red iron oxide, no longer to narrate with embodiment one something in common, and difference is:
The purification and impurity removal of a, ferrous sulfate: earlier 9 tons of byproduct ferrous sulfate of titanium dioxide are imported in the container of belt stirrer, the percentage composition of ferrous sulfate is 85%, starting agitator stirs, constantly add entry in the whipping process, it is fully dissolved, adjust the degree Beaume to 20 of solution, put into the polyacrylamide that accounts for ferrous sulfate total amount 0.3% then, stir, static 4 hours, static back gained supernatant liquid is the copperas solution after purifying;
B, step a gained clear liquid copperas solution is extracted in the container of another belt stirrer, starts agitator and stir, in whipping process, slowly add concentration and be 18% ammoniacal liquor, it is fully reacted, when the pH of solution value is 7, stop to add ammoniacal liquor, i.e. reaction stops;
C, step b gained material is washed, filters, treat that pH value of filtrate is to stop at 7 o'clock, obtain filter cake and filtrate, gained ammonium sulfate filtrate is concentrated, directly supply with composite fertilizer factory as raw material when degree Beaume is 22 when filtrate is concentrated to;
D, step c gained filter cake is calcined with rotary kiln, calcining temperature is 800 ℃, and calcination time is 5 hours, obtains the work in-process red iron oxide after the calcining;
E, steps d gained work in-process are put into ball mill and added entry, the weight ratio that work in-process red iron oxide and water add is 1: 0.8, ball milling 1.2 hours, behind the ball milling gained material is washed, filtered, adopt the rotary kiln snead process to dry then, bake out temperature is 180 ℃, and drying time is 1.5 hours, after the oven dry it is crushed to and promptly gets the red iron oxide product more than 320 orders, through weighing 1.98 tons of gained red iron oxides.
Embodiment three: a kind of method of utilizing byproduct ferrous sulfate of titanium dioxide to prepare red iron oxide, no longer to narrate with embodiment one something in common, and difference is:
The purification and impurity removal of a, ferrous sulfate: earlier 9 tons of byproduct ferrous sulfate of titanium dioxide are imported in the container of belt stirrer, the percentage composition of ferrous sulfate is 88%, starting agitator stirs, constantly add entry in the whipping process, it is fully dissolved, adjust the degree Beaume to 25 of solution, put into the polyacrylamide that accounts for ferrous sulfate total amount 0.5% then, stir, static 2 hours, static back gained supernatant liquid is the copperas solution after purifying;
B, step a gained clear liquid copperas solution is extracted in the container of another belt stirrer, starts agitator and stir, in whipping process, slowly add concentration and be 20% ammoniacal liquor, it is fully reacted, when the pH of solution value is 7.5, stop to add ammoniacal liquor, i.e. reaction stops;
C, step b gained material is washed, filters, treat that pH value of filtrate is to stop at 7 o'clock, obtain filter cake and filtrate, gained ammonium sulfate filtrate is concentrated, directly supply with composite fertilizer factory as raw material when degree Beaume is 20 when filtrate is concentrated to;
D, step c gained filter cake is calcined with rotary kiln, calcining temperature is 750 ℃, and calcination time is 5 hours, obtains the work in-process red iron oxide after the calcining;
E, steps d gained work in-process are put into ball mill and added entry, the weight ratio that work in-process red iron oxide and water add is 1: 1, ball milling 1.5 hours, behind the ball milling gained material is washed, filtered, adopt the rotary kiln snead process to dry then, bake out temperature is 190 ℃, and drying time is 1 hour, after the oven dry it is crushed to and promptly gets the red iron oxide product more than 320 orders, through weighing 2.05 tons of gained red iron oxides.
Embodiment four: a kind of method of utilizing byproduct ferrous sulfate of titanium dioxide to prepare red iron oxide, no longer to narrate with embodiment one something in common, and difference is:
The purification and impurity removal of a, ferrous sulfate: earlier 9 tons of byproduct ferrous sulfate of titanium dioxide are imported in the container of belt stirrer, the percentage composition of ferrous sulfate is 92%, starting agitator stirs, constantly add entry in the whipping process, it is fully dissolved, adjust the degree Beaume to 35 of solution, put into the polyacrylamide that accounts for ferrous sulfate total amount 0.8% then, stir, static 6 hours, static back gained supernatant liquid is the copperas solution after purifying;
B, step a gained clear liquid copperas solution is extracted in the container of another belt stirrer, starts agitator and stir, in whipping process, slowly add concentration and be 20% ammoniacal liquor, it is fully reacted, when the pH of solution value is 8, stop to add ammoniacal liquor, i.e. reaction stops;
C, step b gained material is washed, filters, treat that pH value of filtrate is to stop at 7 o'clock, obtain filter cake and filtrate, gained ammonium sulfate filtrate is concentrated, directly supply with composite fertilizer factory as raw material when degree Beaume is 18 when filtrate is concentrated to;
D, step c gained filter cake is calcined with rotary kiln, calcining temperature is 700 ℃, and calcination time is 6 hours, obtains the work in-process red iron oxide after the calcining;
E, steps d gained work in-process are put into ball mill and added entry, the weight ratio that work in-process red iron oxide and water add is 1: 0.6, ball milling 1.3 hours, behind the ball milling gained material is washed, filtered, adopt the rotary kiln snead process to dry then, bake out temperature is 180 ℃, and drying time is 1.5 hours, after the oven dry it is crushed to and promptly gets the red iron oxide product more than 320 orders, through weighing 2.20 tons of gained red iron oxides.
Embodiment five: a kind of method of utilizing byproduct ferrous sulfate of titanium dioxide to prepare red iron oxide, no longer to narrate with embodiment one something in common, and difference is:
The purification and impurity removal of a, ferrous sulfate: earlier 9 tons of byproduct ferrous sulfate of titanium dioxide are imported in the container of belt stirrer, the percentage composition of ferrous sulfate is 90%, starting agitator stirs, constantly add entry in the whipping process, it is fully dissolved, adjust the degree Beaume to 23 of solution, put into the polyacrylamide that accounts for ferrous sulfate total amount 0.2% then, stir, static 4 hours, static back gained supernatant liquid is the copperas solution after purifying;
B, step a gained clear liquid copperas solution is extracted in the container of another belt stirrer, starts agitator and stir, in whipping process, slowly add concentration and be 16% ammoniacal liquor, it is fully reacted, when the pH of solution value is 8.5, stop to add ammoniacal liquor, i.e. reaction stops;
C, step b gained material is washed, filters, treat that pH value of filtrate is to stop at 6.8 o'clock, obtain filter cake and filtrate, gained ammonium sulfate filtrate is concentrated, directly supply with composite fertilizer factory as raw material when degree Beaume is 20 when filtrate is concentrated to;
D, step c gained filter cake is calcined with rotary kiln, calcining temperature is 900 ℃, and calcination time is 3 hours, obtains the work in-process red iron oxide after the calcining;
E, steps d gained work in-process are put into ball mill and added entry, the weight ratio that work in-process red iron oxide and water add is 1: 0.6, ball milling 1.2 hours, behind the ball milling gained material is washed, filtered, adopt the rotary kiln snead process to dry then, bake out temperature is 200 ℃, and drying time is 1 hour, after the oven dry it is crushed to and promptly gets the red iron oxide product more than 320 orders, through weighing 2.1 tons of gained red iron oxides.
Embodiment six: a kind of method of utilizing byproduct ferrous sulfate of titanium dioxide to prepare red iron oxide, no longer to narrate with embodiment one something in common, and difference is:
The purification and impurity removal of a, ferrous sulfate: earlier 9 tons of byproduct ferrous sulfate of titanium dioxide are imported in the container of belt stirrer, the percentage composition of ferrous sulfate is 86%, starting agitator stirs, constantly add entry in the whipping process, it is fully dissolved, adjust the degree Beaume to 28 of solution, put into the polyacrylamide that accounts for ferrous sulfate total amount 0.4% then, stir, static 3 hours, static back gained supernatant liquid is the copperas solution after purifying;
B, step a gained clear liquid copperas solution is extracted in the container of another belt stirrer, starts agitator and stir, in whipping process, slowly add concentration and be 20% ammoniacal liquor, it is fully reacted, when the pH of solution value is 9, stop to add ammoniacal liquor, i.e. reaction stops;
C, step b gained material is washed, filters, treat that pH value of filtrate is to stop at 6.5 o'clock, obtain filter cake and filtrate, gained ammonium sulfate filtrate is concentrated, directly supply with composite fertilizer factory as raw material when degree Beaume is 20 when filtrate is concentrated to;
D, step c gained filter cake is calcined with rotary kiln, calcining temperature is 950 ℃, and calcination time is 3 hours, obtains the work in-process red iron oxide after the calcining;
E, steps d gained work in-process are put into ball mill and added entry, the weight ratio that work in-process red iron oxide and water add is 1: 0.5, ball milling 1.5 hours, behind the ball milling gained material is washed, filtered, adopt the rotary kiln snead process to dry then, bake out temperature is 180 ℃, and drying time is 1.5 hours, after the oven dry it is crushed to and promptly gets the red iron oxide product more than 320 orders, through weighing 2.0 tons of gained red iron oxides.
Embodiment seven: a kind of method of utilizing byproduct ferrous sulfate of titanium dioxide to prepare red iron oxide, no longer to narrate with embodiment one something in common, and difference is:
The purification and impurity removal of a, ferrous sulfate: earlier 9 tons of byproduct ferrous sulfate of titanium dioxide are imported in the container of belt stirrer, the percentage composition of ferrous sulfate is 90%, starting agitator stirs, constantly add entry in the whipping process, it is fully dissolved, adjust the degree Beaume to 33 of solution, put into the polyacrylamide that accounts for ferrous sulfate total amount 0.6% then, stir, static 5 hours, static back gained supernatant liquid is the copperas solution after purifying;
B, step a gained clear liquid copperas solution is extracted in the container of another belt stirrer, starts agitator and stir, in whipping process, slowly add concentration and be 15% ammoniacal liquor, it is fully reacted, when the pH of solution value is 7.5, stop to add ammoniacal liquor, i.e. reaction stops;
C, step b gained material is washed, filters, treat that pH value of filtrate is to stop at 7 o'clock, obtain filter cake and filtrate, gained ammonium sulfate filtrate is concentrated, directly supply with composite fertilizer factory as raw material when degree Beaume is 20 when filtrate is concentrated to;
D, step c gained filter cake is calcined with rotary kiln, calcining temperature is 1000 ℃, and calcination time is 2 hours, obtains the work in-process red iron oxide after the calcining;
E, steps d gained work in-process are put into ball mill and added entry, the weight ratio that work in-process red iron oxide and water add is 1: 1, ball milling 1 hour, behind the ball milling gained material is washed, filtered, adopt the rotary kiln snead process to dry then, bake out temperature is 195 ℃, and drying time is 1 hour, after the oven dry it is crushed to and promptly gets the red iron oxide product more than 320 orders, through weighing 2.12 tons of gained red iron oxides.
Embodiment eight: a kind of method of utilizing byproduct ferrous sulfate of titanium dioxide to prepare red iron oxide, no longer to narrate with embodiment one something in common, and difference is:
The purification and impurity removal of a, ferrous sulfate: earlier 9 tons of byproduct ferrous sulfate of titanium dioxide are imported in the container of belt stirrer, the percentage composition of ferrous sulfate is 90%, starting agitator stirs, constantly add entry in the whipping process, it is fully dissolved, adjust the degree Beaume to 30 of solution, put into the polyacrylamide that accounts for ferrous sulfate total amount 0.2% then, stir, static 2 hours, static back gained supernatant liquid is the copperas solution after purifying;
B, step a gained clear liquid copperas solution is extracted in the container of another belt stirrer, starts agitator and stir, in whipping process, slowly add concentration and be 20% ammoniacal liquor, it is fully reacted, when the pH of solution value is 7.5, stop to add ammoniacal liquor, i.e. reaction stops;
C, step b gained material is washed, filters, treat that pH value of filtrate is to stop at 7 o'clock, obtain filter cake and filtrate, gained ammonium sulfate filtrate is concentrated, directly supply with composite fertilizer factory as raw material when degree Beaume is 20 when filtrate is concentrated to;
D, step c gained filter cake is calcined with rotary kiln, calcining temperature is 850 ℃, and calcination time is 4 hours, obtains the work in-process red iron oxide after the calcining;
E, steps d gained work in-process are put into ball mill and added entry, the weight ratio that work in-process red iron oxide and water add is 1: 0.6, ball milling 1.2 hours, behind the ball milling gained material is washed, filtered, adopt the rotary kiln snead process to dry then, bake out temperature is 185 ℃, and drying time is 1.5 hours, after the oven dry it is crushed to and promptly gets the red iron oxide product more than 320 orders, through weighing 2.08 tons of gained red iron oxides.
Claims (8)
1. method of utilizing byproduct ferrous sulfate of titanium dioxide to prepare red iron oxide, described method is to be raw material with the by-product ferrous sulfate during that produces in the production process of titanium pigment, earlier with its purification and impurity removal, make further prepared in reaction with the copperas solution after purifying then and become the red iron oxide product, it is characterized in that:
The purification and impurity removal of a, ferrous sulfate: earlier byproduct ferrous sulfate of titanium dioxide is imported in the container of belt stirrer and stir, constantly add entry in the whipping process, it is fully dissolved, the degree Beaume of adjusting solution is 20～35, put into flocculation agent then, the add-on of flocculation agent is 0.1～0.8% of a ferrous sulfate gross weight, stirring, static more than 2 hours, and static back supernatant liquid is the copperas solution after purifying;
B, step a gained clear liquid copperas solution is extracted in the container of another belt stirrer and stirs, slowly add ammoniacal liquor in whipping process, the concentration of ammoniacal liquor is 15～20%, it is fully reacted, when the pH of solution value is 6.5～9, stop to add ammoniacal liquor, i.e. reaction stops;
C, step b gained material is washed, filters, treat that pH value of filtrate is to stop, and obtains filter cake and filtrate at 6.5～7 o'clock;
D, step c gained filter cake is calcined with kiln, continuous bubbling air in calcination process, calcining temperature is 700～1000 ℃, calcination time is 2～6 hours, obtains the work in-process red iron oxide after the calcining;
E, steps d gained work in-process red iron oxide is put into ball mill and added entry, the weight ratio that work in-process red iron oxide and water add is 1: 0.5～1, ball milling 1～2 hour, behind the ball milling gained material is washed, filtered and dries, bake out temperature is 180～200 ℃, drying time is 1～1.5 hour, is crushed to after the oven dry and promptly gets the red iron oxide product more than 320 orders.
2. a kind of method of utilizing byproduct ferrous sulfate of titanium dioxide to prepare red iron oxide according to claim 1 is characterized in that: the percentage composition of ferrous sulfate is 85～92% in the described byproduct ferrous sulfate of titanium dioxide.
3. a kind of method of utilizing byproduct ferrous sulfate of titanium dioxide to prepare red iron oxide according to claim 1 is characterized in that: the stirring velocity of agitator described in the step a is 30 rev/mins～42 rev/mins; Described flocculation agent is a polyacrylamide, and its molecular weight is 3,000,000, and consumption calculates by 100% polyacrylamide.
4. a kind of method of utilizing byproduct ferrous sulfate of titanium dioxide to prepare red iron oxide according to claim 1, it is characterized in that: the container bottom residual precipitate of static back described in the step a enters in the useless vice processing pond of red iron oxide in producing, and focuses on qualified discharge.
5. a kind of method of utilizing byproduct ferrous sulfate of titanium dioxide to prepare red iron oxide according to claim 1 is characterized in that: the stirring velocity of agitator described in the step b is 30 rev/mins～42 rev/mins; Described pH value is 6.5～7.5.
6. a kind of method of utilizing byproduct ferrous sulfate of titanium dioxide to prepare red iron oxide according to claim 1, it is characterized in that: filtrate described in the step c is ammoniumsulphate soln, is that 18～22 o'clock direct composite fertilizer factories that supply with are as raw material with its evaporation concentration to degree Beaume.
7. a kind of method of utilizing byproduct ferrous sulfate of titanium dioxide to prepare red iron oxide according to claim 1 is characterized in that: kiln described in the steps d adopts rotary kiln, and described calcining temperature is 800～900 ℃.
8. a kind of method of utilizing byproduct ferrous sulfate of titanium dioxide to prepare red iron oxide according to claim 1 is characterized in that: the rotary kiln snead process is adopted in oven dry described in the step e; Described water lotion through washing returns step a and recycles.
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| CN102092794B (en) * | 2010-12-08 | 2012-08-08 | 浙江大学 | Preparation method of nano iron oxide yellow or nano iron oxide red |
| CN102344169B (en) * | 2011-06-28 | 2013-06-19 | 广西地博矿业集团股份有限公司 | Method for producing iron-enriched ore by using ferrous sulfate heptahydrate |
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