CN101016172A - Preparing process for nano alpha-Fe2O3 by glycerin atmosphere pressure crystallization method - Google Patents
Preparing process for nano alpha-Fe2O3 by glycerin atmosphere pressure crystallization method Download PDFInfo
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- CN101016172A CN101016172A CN 200610041767 CN200610041767A CN101016172A CN 101016172 A CN101016172 A CN 101016172A CN 200610041767 CN200610041767 CN 200610041767 CN 200610041767 A CN200610041767 A CN 200610041767A CN 101016172 A CN101016172 A CN 101016172A
- Authority
- CN
- China
- Prior art keywords
- glycerol
- fe2o3
- glycerine
- anhydrous
- under
- 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.)
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- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 title claims abstract description 105
- 235000011187 glycerol Nutrition 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 7
- 229910003145 α-Fe2O3 Inorganic materials 0.000 title abstract 3
- 238000002425 crystallisation Methods 0.000 title description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 10
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 238000005516 engineering process Methods 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 4
- 239000004568 cement Substances 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000013078 crystal Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 239000000084 colloidal system Substances 0.000 claims description 2
- 238000000354 decomposition reaction Methods 0.000 claims description 2
- 239000003995 emulsifying agent Substances 0.000 claims description 2
- 230000003472 neutralizing effect Effects 0.000 claims description 2
- 239000012266 salt solution Substances 0.000 claims description 2
- 238000009826 distribution Methods 0.000 claims 1
- 238000013021 overheating Methods 0.000 claims 1
- 239000000546 pharmaceutical excipient Substances 0.000 claims 1
- 239000000843 powder Substances 0.000 claims 1
- 238000002360 preparation method Methods 0.000 claims 1
- 238000000197 pyrolysis Methods 0.000 claims 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 4
- 238000004064 recycling Methods 0.000 abstract description 4
- 239000002253 acid Substances 0.000 abstract description 3
- 239000006227 byproduct Substances 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract description 3
- 239000000047 product Substances 0.000 abstract description 3
- 229910021529 ammonia Inorganic materials 0.000 abstract description 2
- 150000003863 ammonium salts Chemical class 0.000 abstract description 2
- 239000002002 slurry Substances 0.000 abstract 2
- 230000001804 emulsifying effect Effects 0.000 abstract 1
- 230000003311 flocculating effect Effects 0.000 abstract 1
- 239000004816 latex Substances 0.000 abstract 1
- 229920000126 latex Polymers 0.000 abstract 1
- 238000003825 pressing Methods 0.000 abstract 1
- 238000007789 sealing Methods 0.000 abstract 1
- 239000013049 sediment Substances 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 28
- 235000019441 ethanol Nutrition 0.000 description 6
- 229910052742 iron Inorganic materials 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- JDBBTVFYDZWUFI-UHFFFAOYSA-K iron(3+) trinitrite Chemical compound [Fe+3].[O-]N=O.[O-]N=O.[O-]N=O JDBBTVFYDZWUFI-UHFFFAOYSA-K 0.000 description 1
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(III) nitrate Inorganic materials [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 1
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- NJTGANWAUPEOAX-UHFFFAOYSA-N molport-023-220-454 Chemical compound OCC(O)CO.OCC(O)CO NJTGANWAUPEOAX-UHFFFAOYSA-N 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 150000005837 radical ions Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Compounds Of Iron (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a new manufacturing technique of nanometer alpha-Fe2O3 through pressing glycerine under normal pressure, which comprises the following steps: 1. making high-purity liquid of Fe3+ salt; 2. reacting excessive ammonia and Fe3+ liquid to make Fe (OH) 3 latex; insulating the flocculating sediment; filtering Fe (OH) 3; rinsing through pure water; emulsifying with glycerine evenly; heating to dehydrate; obtaining Fe (OH) 3 gel; 3. isotroping; adding into high-temperature heat autoclave; sealing; obtaining Fe2O3 glycerine slurry; draining steam; 4. heating anhydrous Fe2O3 glycerine slurry under 0.2atm at 240-260 deg.c; recycling glycerine through condenser; recycling alpha-Fe2O3 nanometer product; 5. recycling reacting mother liquid; adding acid to neutralize; dehydrating; obtaining the by-product of ammonium salt.
Description
(I) technical field
The invention provides a production technology of inorganic chemical products, in particular to a nano α -Fe by glycerol normal pressure crystallization2O3A production technology.
(II) technical background
Production of nano α -Fe2O3A supercritical crystallizing process for preparing the representative alcohol from Fe by ammonia water neutralization3+High purity salt solution to obtain Fe (OH)3↓, filtering, rinsing with pure water, washing with absolute ethyl alcohol, replacing Fe (OH)3The cement contains water to obtain ethanol Fe (OH)3Gel is put into a high-pressure kettle, dried at the temperature of more than or equal to 260 ℃ under the pressure of 8MPa, dehydrated and dehydrated to obtain the nanometer α -Fe2O3And (5) producing the product. The process has the advantages of large ethanol consumption, large byproduct mass ethanol containing washing water, dehydration and regeneration, large investment, trouble, high energy consumption, flammability and explosiveness, dehydration and dealcoholization under 8MPa, belongs to supercritical crystallization, and has expensive equipment and complex technology, so the process has high cost and difficult large scale.
The invention uses glycerin (glycerol) to replace ethanol, and glycerin is added to filter out water-containing Fe (OH)3A daub of glycerin and Fe (OH) repeatedly emulsified3Mixing with molecular grade, vacuum concentrating at low temperature to remove free water to obtain anhydrous glycerol Fe (OH)3Homogenizing the daub, and removing the bound water at a temperature of more than or equal to 260 DEG C Boiling point of glycerin is 290 ℃ under normal pressure, and Fe is generated at the moment2O3Still in the glycerol molecule, when the glycerol is heated to more than or equal to 290 ℃ and is vaporized, the content of Fe is reduced2O3The melting point is very high, the nano α -Fe can not be agglomerated at about 290 ℃ at all, and the nano α -Fe is produced2O3Twomajor keys are: highly dispersed and nano Fe-proof2O3The crystal grains grow up and are agglomerated, the addition of the glycerol can be ensured at the same time, the boiling point of the glycerol is higher than that of the ethanol, the dielectric constant is large, the agglomeration resistance is better, the vapor condensation and recovery are simple, the energy is saved, the operation is carried out under normal pressure, the equipment can be self-made, and the large-scale production is not difficult.
Disclosure of the invention
The process of the invention is that ① produces Fe3+Salt high-purity liquid: FeCl3、Fe2(SO4)3、Fe(NO3)3And the like, wherein Fe (NO)3)3The salt has the best effect, and FeCO can be used3Or iron filings as raw material is reacted with excessive nitric acid to produce ferric nitrite, which is then fine filtered to remove dregs, because the iron filings are reduced and substituted by Ni, Co, Cu and Pb, etc. and most of the alloy components of C, Si, P and S in iron can be removed simultaneously, Al and Mn can be absorbed by ion exchanger to obtain purified Fe (NO)3)2After the solution is treated, under the action of excessive nitric acid, blowing purified air or adding hydrogen peroxide to oxidize into Fe (NO)3)3Liquid with concentration controlled at about 0.6mol/L, ② Fe3+The salt high-purity liquid is controlled within 35 +/-2 ℃, ammonia water with the concentration of 16-20 percent and N are added under strong stirring2Preferably, the pH value of the reaction is 9 +/-0.5 under protection, and a small amount of polymer is addedAcrylamide (20 g/m)3) Stirring for 20 min, standing for a day and night, filtering out precipitate, and purifying water to remove acid radical ions to obtain Fe (OH)3Aqueous cement ③ glycerol in aqueous Fe (OH)3In the cement, the anhydrous glycerin is Fe (OH)3Homogenizing for 3-4 times (ultrasonic emulsifier, colloid mill, etc.) with homogenizer, adding into vacuum concentrator, concentrating under 0.2 atmospheric pressure to remove free water to obtain anhydrous glycerol Fe (OH)3Gel ④ anhydrous Glycerol Fe (OH)3Passing the gel through a homogenizer for 3 times, placing into a hot medium kettle, heating with heat-conducting oil or salt bath, or heating with electricity, medium frequency electricity, or far infrared ray, etc., heating the gel in the kettle to 260 deg.C or higher, and reacting for 1 hr under heat preservation to obtain the final product (vapor) reaction, wherein the boiling point of glycerol at normal pressure is 290 ℃, the viscosity at normal temperature is high, the viscosity at 120 ℃ and 260 ℃ is low, and Fe (OH)3The molecules are pyrolyzed under the surrounding of glycerol molecules and are dehydrated into α -Fe2O3No agglomeration and no crystal growth at this temperature, releasing vaporized water, heating to 240-260 deg.C under 0.2 atmospheric pressure, vaporizing glycerol, passing glycerol vapor through a condenser, recovering liquid glycerol for reuse, vaporizing glycerol under negative pressure to prevent decomposition of local superheated glycerol, recovering liquid glycerol containing small amount of α -Fe2O3The particles are red, do not affect the recycling, and are cooled and recovered with α -Fe2O3⑤ recovering mother liquid, neutralizing ammonia with acid to neutrality, concentrating, dewatering and crystallizing to obtain ammonium salt as by-product α -Fe2O3The particle size is adjustable between 10 nm and 500 nm.
Claims (1)
- Glycerol process nanometer α -Fe2O3The new production technology comprises the following steps:①Fe3+the preparation of high-purity salt solution belongs to the existing technology;② neutralizing with ammonia water to prepare Fe (OH)3The two or more than two of the obtained water-containing cement areIn the prior art, protection is not needed;③ Glycerol in aqueous Fe (OH)3Daubing with anhydrous glycerin of Fe (OH)3Homogenizing for 3-4 times (ultrasonic emulsifier or colloid mill) with homogenizer at weight ratio of 25%, adding into vacuum concentrator, concentrating under 0.2 atmospheric pressure to remove free water to obtain anhydrous glycerol Fe (OH)3Gelling;④ Glycerol anhydrous Fe (OH)3Homogenizing for 3 times, loading into pyrolysis kettle, heating to 260 deg.C or higher, and reacting for 1 hr to obtain gelThe reaction is thorough, water vapor is discharged, the temperature is raised to 240-260 ℃ under the atmospheric pressure of less than 0.2, the glycerol is vaporized to the full extent, the glycerol vapor is pumped out of a condenser and recycled to regenerate liquid glycerol for circulation, the glycerol is vaporized under negative pressure, the boiling point is reduced, the overheating decomposition of local glycerol is prevented, and α -Fe of the glycerol is removed to the full extent2O3The nanometer powder has controllable granularity of 10-500nm, narrow particle size distribution, different excipient and controllable crystal form, and theprocess is superior to supercritical alcohol crystallizing process.The above four requests are protected for intellectual property rights.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610041767 CN101016172A (en) | 2006-02-09 | 2006-02-09 | Preparing process for nano alpha-Fe2O3 by glycerin atmosphere pressure crystallization method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610041767 CN101016172A (en) | 2006-02-09 | 2006-02-09 | Preparing process for nano alpha-Fe2O3 by glycerin atmosphere pressure crystallization method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101016172A true CN101016172A (en) | 2007-08-15 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200610041767 Pending CN101016172A (en) | 2006-02-09 | 2006-02-09 | Preparing process for nano alpha-Fe2O3 by glycerin atmosphere pressure crystallization method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101016172A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102115211A (en) * | 2011-01-04 | 2011-07-06 | 华南理工大学 | Nano iron trioxide water-soluble colloid and preparation method thereof |
| CN106395913A (en) * | 2016-08-26 | 2017-02-15 | 天津大学 | A kind of ferromagnetic nano α-Fe2O3 with iron defect and preparation method thereof |
-
2006
- 2006-02-09 CN CN 200610041767 patent/CN101016172A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102115211A (en) * | 2011-01-04 | 2011-07-06 | 华南理工大学 | Nano iron trioxide water-soluble colloid and preparation method thereof |
| CN102115211B (en) * | 2011-01-04 | 2012-12-05 | 华南理工大学 | Preparation method of nano iron trioxide water-soluble colloid |
| CN106395913A (en) * | 2016-08-26 | 2017-02-15 | 天津大学 | A kind of ferromagnetic nano α-Fe2O3 with iron defect and preparation method thereof |
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|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |