CN1415664A - Method for preparing nano iron oxide yellow - Google Patents
Method for preparing nano iron oxide yellow Download PDFInfo
- Publication number
- CN1415664A CN1415664A CN 02137552 CN02137552A CN1415664A CN 1415664 A CN1415664 A CN 1415664A CN 02137552 CN02137552 CN 02137552 CN 02137552 A CN02137552 A CN 02137552A CN 1415664 A CN1415664 A CN 1415664A
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- CN
- China
- Prior art keywords
- iron oxide
- yellow
- oxide yellow
- nano
- preparing
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- 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.)
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 238000000034 method Methods 0.000 title claims description 33
- 239000013078 crystal Substances 0.000 claims abstract description 20
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 6
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims abstract description 5
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims abstract description 5
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 19
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 claims description 13
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 12
- 229910052760 oxygen Inorganic materials 0.000 claims description 12
- 239000001301 oxygen Substances 0.000 claims description 12
- 235000010215 titanium dioxide Nutrition 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 8
- 239000006227 byproduct Substances 0.000 claims description 7
- 239000011734 sodium Substances 0.000 claims description 6
- 239000000654 additive Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- 241000231392 Gymnosiphon Species 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- 230000012010 growth Effects 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims 2
- QERYCTSHXKAMIS-UHFFFAOYSA-M thiophene-2-carboxylate Chemical compound [O-]C(=O)C1=CC=CS1 QERYCTSHXKAMIS-UHFFFAOYSA-M 0.000 claims 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 abstract 4
- 229910000029 sodium carbonate Inorganic materials 0.000 abstract 2
- 235000017550 sodium carbonate Nutrition 0.000 abstract 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 abstract 1
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 239000004408 titanium dioxide Substances 0.000 description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 235000003891 ferrous sulphate Nutrition 0.000 description 3
- 239000011790 ferrous sulphate Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 229910002588 FeOOH Inorganic materials 0.000 description 2
- 230000004323 axial length Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000010954 inorganic particle Substances 0.000 description 2
- 239000001034 iron oxide pigment Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000000877 morphologic effect Effects 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000001052 yellow pigment Substances 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 238000006887 Ullmann reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229960002089 ferrous chloride Drugs 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000012629 purifying agent Substances 0.000 description 1
- 230000035040 seed growth Effects 0.000 description 1
- 239000003516 soil conditioner Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Compounds Of Iron (AREA)
Abstract
A process for preparing nano-class iron oxide yellow from refined FeSO4 includes such steps as adding sodium hexametaphosphate and alkylphenol polyoxyvinylether to the solution of refined FeSo4 while stirring, dropping 10% Na2CO3 solution to make pH=3.5-6.5, introducing O2 gas, reaction at 20-40 deg.C to obtain crystal seeds, introducing O2 gas at 50-60 deg, dropping Na2CO3 solution to make pH=3.0-5.5, reaction for 8 hr to grow crystal, filter, drying and pulverizing.
Description
Technical Field
The invention discloses a preparation method for preparing nano iron oxide yellow, belonging to the field of compound preparation processes.
Background
The nano iron oxide yellow has transparent and bright coloring effect and strong light resistance and weather resistance, has wide application in the fields of car high-grade flash paint coating, printing ink, plastics, food, medicine, cosmetics and the like, and is an important precursor for synthesizing other nano iron oxide pigments and iron magnetic materials. As a nano inorganic particle material with strong functionality, the performance and the morphological structure of the nano inorganic particle material are closely related, including the size and the distribution, the crystal structure, the hue and the like.
There are various methods for preparing iron oxide yellow. In Ullmanns encyclopedie der technischen Chemie (5th Edition, Volume A20, p297), a process for preparing iron oxide yellow is described, using as starting material ferrous sulfate obtained in the pickling of steel sheets, or ferrous sulfate obtained in the production of titanium dioxide by the sulfate process; for example, chinese patents CN1056668, CN1125196 and CN1143611, respectively provide a method for preparing iron oxide yellow by using acid pickling waste liquid, iron-containing waste residue and roasting residue for producing sulfuric acid; further, for example, DE31-19652953.0 provides a process for preparing iron oxide yellow, preferably from ferrous chloride in waste liquors. All the above methods are used for preparing common iron oxide yellow pigments without involving control of the morphological structure of the nano-iron oxide yellow. In addition, german patent DE19812260 provides a process for preparing iron oxide yellow pigments after purifying the copperas, by-product of titanium dioxide production by the sulfuric acid process, but cannot be used for the production of nano-iron oxide yellow. Japanese patent JP2001240500 relates to a method for preparing nano iron oxide yellow by using high-purity ferrous iron as a raw material, and a purified sulfuric acidmethod titanium dioxide byproduct copperas is not used.
Titanium dioxide is an important chemical raw material closely related to national economy, titanium dioxide is mainly produced by a sulfuric acid method in China, a large amount of waste byproducts are generated in the production process, according to statistics, one ton of titanium dioxide is produced by the sulfuric acid method, 3-4 tons of ferrous sulfate (copperas) solid is discharged, and if the titanium dioxide is directly discharged without treatment, the environment is seriously polluted; however, the traditional use of the titanium white byproduct copperas, such as the use as a water purifying agent, a fertilizer, a soil conditioner, a common iron oxide pigment and the like, has low added value of products and low economic benefit, and the resource should be fully utilized.
The invention aims to prepare the nano iron oxide yellow with high added value by using the byproduct copperas produced by titanium dioxide in the sulfuric acid process. Another object of the present invention is to provide a method for preparing nano iron oxide yellow by controlling the process parameters of the seed crystal formation and growth process.
The object of the invention is achieved by a process which uses purified copperas as raw material and is characterized in that a certain amount of mixed additives of sodium hexametaphosphate and OP-10 are added to refined FeSO at a certain temperature and stirring speed4Solutions ofIn the preparation, 10% of Na is added dropwise2CO3The solution is adjusted to pH value of 3.5-6.5, and a certain reaction temperature is kept at 20-40 ℃; then at 0.12-0.18m3Introducing oxygen for reaction under the oxygen flow rate of/h to prepare nano iron oxide yellow crystal seeds; then heating to 50-60 deg.C, and heatingto 0.12-0.18m3Introducing oxygen at the flow rate of/h, and dropwise adding 10% of Na into the solution containing the seed crystal2CO3And (3) maintaining the pH value of the system within the range of 3.0-5.5, reacting for 8 hours to grow seed crystals, and after the reaction is finished, filtering, drying and crushing the suspension containing the nano iron oxide yellow to obtain nano iron oxide yellow particles.
The method mainly controls the hue, the crystal form and the size of the particles by adjusting the process parameters of the forming and growing process of the nano iron yellow crystal seeds, such as pH value, temperature, oxygen flow, stirring speed, additives and other conditions.
The method has the advantages and effects that:
1) the by-product copperas produced by the titanium white production by the sulfuric acid method is used as the raw material, so that the environmental pollution can be eliminated, and the method has obvious social and economic benefits.
2) The method for preparing the nano iron oxide yellow has simple process and easy control, belongs to liquid phase reaction at normal temperature and normal pressure, and is easy to expand to the industrial production scale.
3) The product quality is stable, and the prepared nano iron oxide yellow has small particle size, uniform distribution and good dispersibility.
The method of the invention has the main chemical reaction formula as follows: 1) seed preparation
Thenano iron oxide yellow prepared by the method is bright in color, is analyzed and observed by an X-ray diffractometer, has a crystal form of α -FeOOH structure, is in a spindle shape or a needle shape by utilizing an electron lens to observe, and has the radial length of 100-120nm and the axial length of 20-40 nm.
Specific embodiments of the present invention are described below.
Example 1
400ml of purified FeSO with a concentration of 15% (g/g) are taken4Solution (wherein Mn)2+Less than 0.065% of Ti4+The content is less than 0.01 percent), 0.013g/L sodium hexametaphosphate and 0.020g/LOP-10 mixed additive are added at the stirring speed of 150-250rpm and the temperature of 25-35 ℃, and 10 percent of Na is added2CO3The pH value of the solution is 5.5-6.5, and the solution is 0.16m3Introducing oxygen at the flow rate of/h, and reacting at the temperature of 25-35 ℃ to prepare nano iron oxide yellow seed crystals; then the temperature is raised to 55 ℃ again, and then the temperature is increased to 0.16m3Introducing oxygen at the flow rate of/h, and dropwise adding 10% of Na into the solution containing the seed crystal2CO3Liquid, maintaining the pH value at5.5, reacting for 8 hours to enable the seed crystal to grow, after the reaction is finished, filtering, drying and crushing the suspension containing the nano iron oxide yellow to obtain the nano iron oxide yellow particles which are bright yellow, have a crystal form of α -FeOOH structure, and have good particle dispersibility, the radial length of the particles is 100-120nm, and the axial length of the particles is 20-40 nm.
Claims (5)
1. A process for preparing nano iron oxide yellow from refined and purified copperas includes such steps as adding sodium hexametaphosphate and alkylphenol polyethenoxy ether (OP-10) to refined FeSO at a certain temp and stirring speed4To the solution, 10% Na was added dropwise2CO3The solution is adjusted to the pH value within the range of 3.5-6.5, and a certain reaction temperature is kept; then, oxygen is introduced at a certain speed to react, and the nano iron oxide yellow seed crystal is prepared. Then, at a certain temperature of 20-40 ℃, and thenAt 0.12-0.18m3Introducing oxygen for reaction under the oxygen flow rate of/h to prepare nano iron oxide yellow crystal seeds; then heating to 50-60 deg.C, and heating to 0.12-0.18m3Introducing oxygen at the flow rate of/h, and dropwise adding 10% of Na into the solution containing the seed crystal2CO3Maintaining a certain pH value of the system within a range of 3.0-5.5, and reacting for 8 hours to grow seed crystals; and after the reaction is finished, filtering, drying and crushing the suspension containing the nano iron oxide yellow to obtain nano iron oxide yellow particles.
2. The method as claimed in claim 1, wherein the temperature is 25-35 ℃, the stirring speed is 150-250rpm, the concentration of the mixed additive is 0.013g/l sodium hexametaphosphate and 0.020g/l OP-10.
3. The method as claimed in claim 1, wherein the optimum p value for preparing the nano yellow iron oxide seed crystal is 5.5-6.5, the optimum reaction temperature is 25-35 ℃, and the optimum oxygen flow rate is 0.16m3/h。
4. The method for preparing nanometer yellow iron oxide as claimed in claim 1, wherein the optimal pH value of the seed crystal of the nanometer yellow iron oxide is 5.5 during the growth of its variety, and the optimal oxygen flow rate is 0.16m3The optimum reaction temperature is 55 ℃.
5. The method for preparing nano yellow iron oxide according to claim 1, wherein the FeSO is refined4The source of the method is the byproduct copperas generated in the process of preparing titanium white by a sulfuric acid method, and the material is obtained by purifying the copperas by a certain process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02137552 CN1245458C (en) | 2002-10-21 | 2002-10-21 | Method for preparing nano iron oxide yellow |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02137552 CN1245458C (en) | 2002-10-21 | 2002-10-21 | Method for preparing nano iron oxide yellow |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1415664A true CN1415664A (en) | 2003-05-07 |
| CN1245458C CN1245458C (en) | 2006-03-15 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02137552 Expired - Fee Related CN1245458C (en) | 2002-10-21 | 2002-10-21 | Method for preparing nano iron oxide yellow |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1245458C (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100432156C (en) * | 2005-04-30 | 2008-11-12 | 河南黄河旋风股份有限公司 | Process for preparing nano iron oxide yellow pigment |
| CN105670345A (en) * | 2016-01-05 | 2016-06-15 | 萧县金鹭纺织品有限公司 | Preparation method of flame retardant medium temperature resistant iron oxide yellow pigment |
| CN106000230A (en) * | 2016-07-27 | 2016-10-12 | 升华集团德清华源颜料有限公司 | High-pressure reaction vessel special for preparation of low-length/diameter-ratio iron oxide yellow |
| CN107640790A (en) * | 2017-11-15 | 2018-01-30 | 成都先进金属材料产业技术研究院有限公司 | The method that titanium white by product thing prepares high-purity ferrous sulfate crystal |
| CN113104901A (en) * | 2021-04-13 | 2021-07-13 | 江西理工大学 | Method for preparing iron oxide yellow from rare earth waste acid leaching residues |
| CN113292103A (en) * | 2021-05-25 | 2021-08-24 | 永兴朗丰色料实业有限公司 | Method for producing nano iron oxide red by utilizing solid waste |
| CN117326597A (en) * | 2023-08-30 | 2024-01-02 | 宁波爱诗化妆品有限公司 | Method for regulating and controlling size of nano iron oxide yellow, nano iron oxide yellow and application thereof |
-
2002
- 2002-10-21 CN CN 02137552 patent/CN1245458C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100432156C (en) * | 2005-04-30 | 2008-11-12 | 河南黄河旋风股份有限公司 | Process for preparing nano iron oxide yellow pigment |
| CN105670345A (en) * | 2016-01-05 | 2016-06-15 | 萧县金鹭纺织品有限公司 | Preparation method of flame retardant medium temperature resistant iron oxide yellow pigment |
| CN106000230A (en) * | 2016-07-27 | 2016-10-12 | 升华集团德清华源颜料有限公司 | High-pressure reaction vessel special for preparation of low-length/diameter-ratio iron oxide yellow |
| CN107640790A (en) * | 2017-11-15 | 2018-01-30 | 成都先进金属材料产业技术研究院有限公司 | The method that titanium white by product thing prepares high-purity ferrous sulfate crystal |
| CN113104901A (en) * | 2021-04-13 | 2021-07-13 | 江西理工大学 | Method for preparing iron oxide yellow from rare earth waste acid leaching residues |
| CN113104901B (en) * | 2021-04-13 | 2024-02-09 | 江西理工大学 | Method for preparing iron oxide yellow from rare earth waste acid leaching slag |
| CN113292103A (en) * | 2021-05-25 | 2021-08-24 | 永兴朗丰色料实业有限公司 | Method for producing nano iron oxide red by utilizing solid waste |
| CN117326597A (en) * | 2023-08-30 | 2024-01-02 | 宁波爱诗化妆品有限公司 | Method for regulating and controlling size of nano iron oxide yellow, nano iron oxide yellow and application thereof |
| CN117326597B (en) * | 2023-08-30 | 2024-05-24 | 宁波爱诗化妆品有限公司 | Method for regulating and controlling size of nano iron oxide yellow, nano iron oxide yellow and application thereof |
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| Publication number | Publication date |
|---|---|
| CN1245458C (en) | 2006-03-15 |
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