CN1193937C - Production process of high-purity ferric oxide for ferrite - Google Patents
Production process of high-purity ferric oxide for ferrite Download PDFInfo
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- CN1193937C CN1193937C CNB011069392A CN01106939A CN1193937C CN 1193937 C CN1193937 C CN 1193937C CN B011069392 A CNB011069392 A CN B011069392A CN 01106939 A CN01106939 A CN 01106939A CN 1193937 C CN1193937 C CN 1193937C
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- acidolysis
- ferrous sulfate
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Abstract
The present invention relates to a method for preparing high purity ferric oxide used for ferrites. By the acidolysis and the hydrolysis of ferrous sulphate of titanium dioxide as byproducts, impurities removed, and the purification is carried out; after the purification, double decomposition of the ferrous sulphate and ammonium bicarbonate happens to generate ferric carbonate; the ferric carbonate is washed, dried and roasted so high purity ferric oxide is prepared. The major raw materials needed by the present invention, namely the ferrous sulphate are easy to obtain and have low price; therefore, the production cost is greatly reduced; besides, the byproducts of titanium dioxide are fully utilized so the present invention is a good item for three waste treatment. The ferric oxide products prepared by the present invention have high purity and good quality; the ferric oxide products are suitable for medium grade and high grade ferrites. The present invention has the advantages of simple preparation process and low energy consumption; thus, the cost is further reduced.
Description
Technical field
The present invention relates to a kind of manufacture method of oxide compound of iron, further be meant a kind of manufacture method of high-purity ferric oxide for ferrite.
Background technology
Ferrite has following three kinds with the existing production method of ferric oxide: 1. (major ingredient is FeCl to iron and steel production employing steel sheet pickling waste liquor
2) form ferric oxide through spray roasting.The ferric oxide cost of this explained hereafter is lower, because pickle solution impurity is more, though in recent years through updating, still can not produce high-purity iron oxide, its product only can be used for, low-grade ferrite.2. with soft steel iron sheet and sulfuric acid reaction generation ferrous sulfate again with the metathesis of carbon ammonium after the iron carbonate roasting method.The ferric oxide quality that this method is produced is good, but cost is higher, and raw material is limited.3. the applicant in once invented in 1997 with the titanium white by product ferrous sulfate after acidolysis hydrolysis, crystallization removal of impurities are purified again with the metathesis of carbon ammonium after the iron carbonate roasting method.The good product quality of this method can be used for middle and high shelves ferrite, but that shortcoming is technical process is longer, owing to adopted Crystallization Procedure to purify, makes energy consumption higher, so production cost increases.This technology transfers the chemical plant, Zhuzhou in February, 1997, has now formed to produce 3000 tons throughput per year.
Summary of the invention
The above-mentioned shortcoming that exists in view of prior art.Purpose of the present invention, be provide that a kind of raw material is easy to get, the matter height is inexpensive, technology is simple and the manufacture method of the high-purity ferric oxide for ferrite that energy consumption is lower.
Solution of the present invention is as follows.Purify through acidolysis hydrolysis impurity elimination with the titanium white by product ferrous sulfate, the ferrous sulfate after the purification generates iron carbonate with the metathesis of carbon ammonium, again iron carbonate is made high purity ferric oxide through washing, drying, roasting; In above-mentioned acidolysis hydrolysis reaction, the addition of water and the ratio of ferrous sulfate are 1-10kg water: the 1kg ferrous sulfate, the ratio of iron sheet add-on and ferrous sulfate is the 0.3-20g iron sheet: the 1kg ferrous sulfate, the acidolysis hydrolysising reacting temperature is controlled at 50-100 ℃, the acidolysis hydrolysis time is 5-20 hour, and acidolysis hydrolysis reaction pH value is controlled at 3-5, adds flocculation agent by its settlement number hour in the intact solution of acidolysis hydrolysis, filtering separation obtains transparent clarifying copperas solution then; This solution and ammonium bicarbonate solution are generated iron carbonate through replacement(metathesis)reaction, ph value of reaction is controlled at 5-8, temperature of reaction is controlled at 30-90 ℃, after replacement(metathesis)reaction is complete, with the separate mode of any routine, from the water slurry shape resultant of reaction, isolate the iron carbonate product, then the remaining water soluble salt of ammonia of water flush away, and with it at 100-130 ℃ of temperature range inner drying, dried iron carbonate carried out in 700-1000 ℃ of scope roasting 4-5 hour and obtained high-purity ferric oxide.
Adopting the needed main raw material ferrous sulfate of the inventive method is the titanium white by product product, and raw material is easy to get and inexpensive, thereby makes the production cost of the inventive method greatly reduce, and deserves to be called a good disposal of three wastes project.With the ferrite iron oxide product that the inventive method makes, purity height, quality is good, is suitable for middle and high shelves ferrite and uses.The method that the inventive method and the applicant have implemented in the chemical plant, Zhuzhou is compared, and its distinguishing feature is to have saved the higher Crystallization Procedure of energy consumption, thereby has characteristics, the especially cost that technology is simple, flow process is short, energy consumption is low, cost descends and reduce about 1/3.
Embodiment
The present invention purifies by acidolysis hydrolysis impurity elimination with the titanium white by product ferrous sulfate, then with the metathesis of carbon ammonium after iron carbonate get high-purity ferric oxide for ferrite through washing, dry, roasting single stage method.The used ferrous sulfate of the present invention is cheap titanium white by product product (ferrous sulfate content about 90%; Titanium 1.2%; Manganese 0.8%), the carbon ammonium is industrial goods (containing N is 17%).Its acidolysis hydrolysising reacting temperature is 50-100 ℃, and when temperature was hanged down, the reaction times will prolong, and production efficiency is low.Reaction times was generally 5-20 hour.The water yield that ferrous sulfate adds should be every 1kg ferrous sulfate adds more than the water 1kg, is preferably every 1kg ferrous sulfate and adds the 1-10kg water yield; The water yield is added few, reacts insufficient, prolongs the reaction times, and production efficiency is low; If the water yield is added too much, the energy consumption of then heating required increases; The used water of the present invention should be highly purified, preferably uses deionized water.The add-on of iron sheet is that every 1kg ferrous sulfate adds the 0.3-20g iron sheet during acidolysis hydrolysis, and iron sheet preferably adopts the soft steel iron sheet.Acidolysis hydrolysis reaction pH value is controlled at more than 3, be advisable with 3-5, otherwise hydrolysis is incomplete.When the acidolysis hydrolyzed PH value is reached home, add flocculation agent by its settlement number hour, filtering separation then, transparent clarifying copperas solution, with this solution and ammonium bicarbonate solution replacement(metathesis)reaction generation iron carbonate, its reaction formula is:
PH value is controlled between the 5-8 in the reaction of carbonate synthesis iron, and temperature of reaction is 30-90 ℃.After replacement(metathesis)reaction was complete, iron carbonate can be collected with the separate mode of any routine, and a kind of economy and effective means are to filter, and filtering separation is opened the FeCO of suspension from the water soup compound of reaction
3Behind the product, the water soluble salt of ammonia that iron carbonate water flush away is remaining, and with it 100～130 ℃ of temperature range dryings.Dried iron carbonate carries out roasting and gets Fe in 700～1000 ℃ of scopes
2O
3, roasting will keep certain hour, so that FeCO
3Decompose and become desirable Fe fully
2O
3Product; Roasting time was generally 4～5 hours, and its reaction formula is:
Below with specific embodiment high-purity ferric oxide for ferrite (Fe of the present invention is described
2O
3) manufacture method, but scope of the present invention is not subjected to the limitation of following examples.
Referring to table 1, finished the one group of experiment that comprises embodiment 1, embodiment 2 and embodiment 3 with processing method of the present invention, in this group experiment, particularly according to aforementioned solution of the present invention, among each embodiment 100 gram ferrous sulfate are dissolved in the 100ml-1000ml deionized water of different amounts, in each embodiment, add the iron sheet of the different amounts of 0.3-20 gram, then 50～100 ℃ of different temperature of each embodiment sample heating are carried out the acidolysis hydrolysis, reaction times is 5～20 hours different time, and acidolysis hydrolysis reaction pH value is controlled at 3～5 different values.The dope filtration that the acidolysis hydrolysis is intact, its filtrate and carbon ammonium carry out replacement(metathesis)reaction and get iron carbonate, and the replacement(metathesis)reaction temperature of each embodiment is controlled at 30～90 ℃ of different values, and the replacement(metathesis)reaction terminal point pH value of each embodiment is 5～8 different values.With this iron carbonate with deionized water wash wherein remaining ammonium salt, and the sample of each embodiment is carried out drying in 100～130 ℃ of different temperature values, the iron carbonate sample of dried each the embodiment gained differing temps in 700～1000 ℃ of scopes again carries out roasting, obtains the high purity ferric oxide (Fe of three kinds of different purity at last
2O
3), the roasting time of each embodiment is controlled at 4～5 hours different time.The above-mentioned various data that comprise this group experiment of three embodiment are all listed in the table 1.But it is pointed out that under the prerequisite that meets aforementioned techniques solution of the present invention the relevant technologies data of the foregoing description also can be done certain modification and adjustment.Also can find out Fe among three embodiment simultaneously from table 1
2O
3Content all more than 99.20%, because of foreign matter content is lower, visible iron oxide product is highly purified.
Referring to table 2, it has listed the data on bulk analysis of the high purity ferric oxide finished product that embodiment 2 obtains at last in the table 1, comprising Fe
2O
3The content of content and several major impurities.
Table 1 that the foregoing description relates to and table 2 are after now being respectively in.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| FeSO 4(g) water (ml) iron sheet (g) acidolysis hydrolysising reacting temperature (℃) acidolysis hydrolysis time (H) acidolysis hydrolysis terminal point pH value metathesis reaction terminal point pH value metathesis reaction temperature (℃) FeCO3Drying temperature (℃) FeCO 3Maturing temperature (℃) FeCO 3Roasting time (H) Fe 2O 3Content | 100 100 1 90 5 4 5.5 30 100 700 5 99.20％ | 100 200 4 70 8 5 7.0 50 130 900 5 99.35％ | 100 400 15 50 10 4 8.0 90 110 1000 4 99.24％ |
Table 2
| Embodiment 2 | Fe 2O 3Content | SiO 2 | TiO 2 | CaO | Al 2O 3 | MgO | MnO | SO 4 2- |
| 99.35％ | 0.005％ | 0.002％ | 0.05％ | 0.008％ | 0.004％ | 0.30％ | 0.03％ |
Claims (3)
1, a kind of manufacture method of high-purity ferric oxide for ferrite, it is characterized in that, purify through acidolysis hydrolysis impurity elimination with the titanium white by product ferrous sulfate, the ferrous sulfate after the purification generates iron carbonate with the metathesis of carbon ammonium, again iron carbonate is made high purity ferric oxide through washing, drying, roasting; In above-mentioned acidolysis hydrolysis reaction, the addition of water and the ratio of ferrous sulfate are 1～10kg water: the 1kg ferrous sulfate, the ratio of iron sheet add-on and ferrous sulfate is 0.3～20g iron sheet: the 1kg ferrous sulfate, the acidolysis hydrolysising reacting temperature is controlled at 50～100 ℃, the acidolysis hydrolysis time is 5～20 hours, and acidolysis hydrolysis reaction pH value is controlled at 3～5, adds flocculation agent by its settlement number hour in the intact solution of acidolysis hydrolysis, filtering separation obtains transparent clarifying copperas solution then; This solution and ammonium bicarbonate solution are generated iron carbonate through replacement(metathesis)reaction, ph value of reaction is controlled at 5～8, temperature of reaction is controlled at 30-90 ℃, after replacement(metathesis)reaction is complete, with the separate mode of any routine, from the water slurry shape resultant of reaction, isolate the iron carbonate product, then the remaining water soluble salt of ammonia of water flush away, and with it at 100～130 ℃ of temperature range inner dryings, dried iron carbonate carried out roasting 4～5 hours and obtains high-purity ferric oxide in 700～1000 ℃ of scopes.
2, the manufacture method of high-purity ferric oxide for ferrite according to claim 1 is characterized in that, it is deionized water that ferrous sulfate carries out the water that the acidolysis hydrolysis added.
3, the manufacture method of high-purity ferric oxide for ferrite according to claim 1 is characterized in that, the iron carbonate of replacement(metathesis)reaction gained is separated with filtering mode, promptly filters to isolate the iron carbonate product of suspension from the water soup compound of reaction.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011069392A CN1193937C (en) | 2001-03-13 | 2001-03-13 | Production process of high-purity ferric oxide for ferrite |
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|---|---|---|---|
| CNB011069392A CN1193937C (en) | 2001-03-13 | 2001-03-13 | Production process of high-purity ferric oxide for ferrite |
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| CN1193937C true CN1193937C (en) | 2005-03-23 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100366544C (en) * | 2005-06-30 | 2008-02-06 | 宝山钢铁股份有限公司 | Iron oxide powder solid purifying process |
| CN100351181C (en) * | 2006-03-24 | 2007-11-28 | 广西冶金研究院 | Method of preparing high purity iron oxide for soft magnet using titanium white by product ferrous sulphate |
| CN105110382A (en) * | 2015-09-22 | 2015-12-02 | 升华集团德清华源颜料有限公司 | Method for preparing high-purity gamma-Fe2O3 iron oxide red pigment |
| CN110129061B (en) * | 2019-05-31 | 2021-02-09 | 北京建工环境修复股份有限公司 | Stabilizer for repairing heavy metal pollution and preparation method and application thereof |
| CN113582238A (en) * | 2021-08-12 | 2021-11-02 | 山东春光磁电科技有限公司 | Preparation method of iron source for manganese-zinc ferrite |
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