CN1009080B - Prepn. of superfine ferrous oxide - Google Patents
Prepn. of superfine ferrous oxideInfo
- Publication number
- CN1009080B CN1009080B CN 87108286 CN87108286A CN1009080B CN 1009080 B CN1009080 B CN 1009080B CN 87108286 CN87108286 CN 87108286 CN 87108286 A CN87108286 A CN 87108286A CN 1009080 B CN1009080 B CN 1009080B
- Authority
- CN
- China
- Prior art keywords
- ferrous sulfate
- reaction
- product
- present
- ferric oxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
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- Compounds Of Iron (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The present invention relates to a method for preparing ultramicro fine iron oxide. Ultramicro fine iron oxide is prepared by that waste materials which contain ferrous sulfate heptahydrate and are discharged in some production processes are processed to obtain ferrous sulfate heptahydrate crystals used as raw materials, and the raw materials and carbonates of alkali metal or alkaline earth metal are thoroughly mixed and are processed through a solid phase reaction. The method of the present invention comprises four technological processes of mixing, reaction, washing and dewatering drying. The maximum grain diameter of a product is 100 nm, the minimum grain diameter of the product is 8 nm, and the average grain diameter of the product is 36 nm. The present invention has an important purpose for industrial fields of electronic telephonic communication, coating pigment preparation, rubber and plastic preparation, and catalyst preparation, etc.
Description
The invention belongs to the compound of metal in the inorganic chemistry, be specifically related to ultra tiny ferric oxide (Fe
2O
3) the preparation method.
Ultra tiny ferric oxide has better characteristic than the ferric oxide of general powder or common micro mist on physicochemical property such as electricity, magnetics, optics and calorifics.It is the important source material of producing ferrite magnetic material in electronics, telecommunication industry; In coatings industry, be used as the pigment powder, particularly make the transparent pigment powder of ultraviolet absorpting film; In rubber, plastics industry, be used as tinting material; In chemical industry, be used as catalyzer or the like, can produce various high-grade goods.Ultra tiny ferric oxide is to have the new type functional inorganic materials that waits to develop development prospect.
In the prior art, English Patent Brit 1,094 is arranged, 900(1967), it adopts volatile salt and bicarbonate of ammonia and ferrous sulfate aqueous solution reaction precipitation to go out FeCO
3, make ferric oxide through washing, dehydration heated oxide under～600 ℃ of airflows again; Japanese kokai publication sho 57-88036 is arranged, and is to adopt yellow soda ash and ferrous salt reaction solution to generate FeCO
3, dewater and make ferric oxide at 250～500 ℃ through atmospheric oxidation, washing, filtration, after dry.They all adopt liquid phase reaction to be settled out FeCO
3, heated oxide makes iron oxide product then, and all is ferric oxide powders of conventional particle diameter.On October 16th, 1985, disclosed Japanese kokai publication sho 60-204629 was with excessive lime carbonate (CaCO
3), join in the waste water that contains ferrous ion, be blown into oxidizing gas, generate ferromagnetism throw out (particle diameter can reach 80nm) in that wastewater temperature is remained under the condition more than 55 ℃; Again this ferromagnetism throw out is reclaimed with electromagnetic separation process; Be heated oxidation (500 ℃) at last and be prepared into ferric oxide.Although adopt this method can obtain the ferromagnetism throw out intermediate that particle diameter is 80nm, the document does not confirm that final product is ultra tiny ferric oxide; In addition, this ferromagnetism throw out also may with CaSO
4Generate mixed crystal, receive impurity such as its contained gypsum, lime carbonate with the electromagnetic method partition method and separate, will acquire a certain degree of difficulty in industrial enforcement.Only have in the world at present Japan on May 9th, 1987 disclosed spy open clear 62-100420, for preparing the patented technology of ultra tiny ferric oxide, its adopts beta-diketon iron complex to carry out vapor phase hydrolysis, obtains high purity rhombohedral iron ore (Fe
2O
3) super-fine powder, median size is less than 50nm.But this technology is used for the restriction that industrial production can be subjected to raw material sources, and the preparation method is also complicated simultaneously.
The objective of the invention is to rationally utilize the sulfur acid ferrous waste material that discharges in some Industrial processes, adopt the easy preparation technology who is different from prior art, the production median size is less than the ultra tiny ferric oxide of 50nm.
Invention is achieved in that
With the sulfur acid ferrous waste material (for example waste material of Producing Titanium Dioxide tankage, preparation iron-containing catalyst, iron and steel pickling waste liquid etc.) that discharges in some Industrial processes, the treated ferrous sulfate crystal (FeSO7H that obtains
2O) be raw material, the well-mixed solid state reaction of the carbonate of employing and basic metal or alkaline-earth metal is produced ultra tiny ferric oxide.It comprises following four technological processs:
1. batch mixing: the ferrous sulfate crystal raw material and the carbonate of basic metal or alkaline-earth metal are pressed mol than 0.9～1.2: 1 fully stirs, and mixes.
2. react: the blended material is packed into to have in the reactor of efficient uniform mixing ability, is having in the presence of the air or oxygen, and 300-600 ℃ of temperature range internal heating reacted 1～4 hour.
Reaction equation is as follows:
3. washing: the reaction product water is carried out repeatedly rinsing, till being washed till in the rinse water sulfate radical-free and existing; And from the rinse water that contain high concentration sulphate, reclaim soluble sulphate.
4. dehydrate: the material filter-press dehydration after will washing places moisture eliminator 100～130 ℃ of temperature range inner dryings 1～4 hour again.Promptly get ultra tiny ferric oxide finished product after dehydrating.
Fig. 1 is a square block diagram of the present invention.
Compared with the prior art the present invention owing to adopted the carbonate and the ferrous sulfate crystalline solid state reaction of basic metal or alkaline-earth metal, is able in high density reactant, carries out the high speed reaction under the high impellent and directly generates Fe
2O
3, both simplified Production Flow Chart, shortened the production cycle, and product is ultra tiny ferric oxide.
By the preparation method of the invention described above, can be with the sulfur acid ferrous waste material that discharges in some Industrial processes, comprehensive utilization is turned waste into wealth, and technological process is easy simultaneously, low, the Functionality, quality and appealing design of product cost.Through the check and analysis of H-600 type electron microscope, be～100nm that minimum grain size is～8nm that median size is～36nm by the prepared ferric oxide powder maximum particle diameter of the present invention; It is spherical that majority is, and minority is shaft-like.Fig. 2 amplifies 100,000 times of photos that detect the prepared ferric oxide of the present invention with H-600 type electron microscope.Affirmation is a kind of super-fine powder material by the prepared ferric oxide powder of the present invention.Therefore, the present invention rationally utilizes the sulfur acid ferrous waste material that discharges in some Industrial processes, produces a desirable approach of ultra tiny ferric oxide new type functional inorganic materials.
Claims (2)
1, a kind of method for preparing ultra tiny ferric oxide, it is to be raw material with the ferrous sulfate crystal, and comprises batch mixing, reaction, washes, dehydrates four technological processs; Feature of the present invention is: said reaction process be one in reactor with efficient uniform mixing ability, having in the presence of the air or oxygen, under 1～4 hour the condition of 300～600 ℃ of temperature range internal heating, use basic metal or the carbonate of alkaline-earth metal and the process that the ferrous sulfate crystal carries out solid state reaction.
2, according to the method for the ultra tiny ferric oxide of the described preparation of claim 1, the carbonate that it is characterized in that ferrous sulfate crystal and basic metal or alkaline-earth metal before solid state reaction by mol than 0.9～1.2: 1 abundant batch mixing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 87108286 CN1009080B (en) | 1987-12-30 | 1987-12-30 | Prepn. of superfine ferrous oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 87108286 CN1009080B (en) | 1987-12-30 | 1987-12-30 | Prepn. of superfine ferrous oxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN87108286A CN87108286A (en) | 1988-07-06 |
| CN1009080B true CN1009080B (en) | 1990-08-08 |
Family
ID=4816463
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 87108286 Expired CN1009080B (en) | 1987-12-30 | 1987-12-30 | Prepn. of superfine ferrous oxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1009080B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1036775C (en) * | 1994-03-16 | 1997-12-24 | 南京化学工业(集团)公司研究院 | Method for preparing high-content iron oxide red pigment from iron-containing industrial cinder |
| CN102181628B (en) * | 2011-03-30 | 2013-02-20 | 攀钢集团有限公司 | Method for producing rich iron ore from ferrous sulfate |
| CN102603009B (en) * | 2012-02-21 | 2014-08-20 | 升华集团德清华源颜料有限公司 | Method for preparing nano transparent ferric oxide red pigment |
-
1987
- 1987-12-30 CN CN 87108286 patent/CN1009080B/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| CN87108286A (en) | 1988-07-06 |
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| CF01 | Termination of patent right due to non-payment of annual fee |