CN1239077A - Solid-phase catalytic oxidizing process for preparing alpha-Fe2O3 - Google Patents
Solid-phase catalytic oxidizing process for preparing alpha-Fe2O3 Download PDFInfo
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- CN1239077A CN1239077A CN 98112890 CN98112890A CN1239077A CN 1239077 A CN1239077 A CN 1239077A CN 98112890 CN98112890 CN 98112890 CN 98112890 A CN98112890 A CN 98112890A CN 1239077 A CN1239077 A CN 1239077A
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- 230000001590 oxidative effect Effects 0.000 title claims 4
- 238000004519 manufacturing process Methods 0.000 title abstract description 14
- 230000003197 catalytic effect Effects 0.000 title abstract description 4
- 239000007790 solid phase Substances 0.000 title abstract description 3
- 229910003145 α-Fe2O3 Inorganic materials 0.000 title 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 20
- 229910052742 iron Inorganic materials 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 10
- 230000003647 oxidation Effects 0.000 claims abstract description 9
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 claims abstract description 7
- 239000003054 catalyst Substances 0.000 claims abstract description 6
- LBSANEJBGMCTBH-UHFFFAOYSA-N manganate Chemical compound [O-][Mn]([O-])(=O)=O LBSANEJBGMCTBH-UHFFFAOYSA-N 0.000 claims abstract description 5
- YQOXCVSNNFQMLM-UHFFFAOYSA-N [Mn].[Ni]=O.[Co] Chemical compound [Mn].[Ni]=O.[Co] YQOXCVSNNFQMLM-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract 2
- 238000006243 chemical reaction Methods 0.000 claims description 6
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 6
- -1 Xiao Suangu Chemical compound 0.000 claims description 4
- OQVYMXCRDHDTTH-UHFFFAOYSA-N 4-(diethoxyphosphorylmethyl)-2-[4-(diethoxyphosphorylmethyl)pyridin-2-yl]pyridine Chemical compound CCOP(=O)(OCC)CC1=CC=NC(C=2N=CC=C(CP(=O)(OCC)OCC)C=2)=C1 OQVYMXCRDHDTTH-UHFFFAOYSA-N 0.000 claims description 3
- BNBLBRISEAQIHU-UHFFFAOYSA-N disodium dioxido(dioxo)manganese Chemical group [Na+].[Na+].[O-][Mn]([O-])(=O)=O BNBLBRISEAQIHU-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 150000002823 nitrates Chemical class 0.000 claims description 3
- 235000010344 sodium nitrate Nutrition 0.000 claims description 3
- 239000004317 sodium nitrate Substances 0.000 claims description 3
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical group CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 claims description 2
- JYLNVJYYQQXNEK-UHFFFAOYSA-N 3-amino-2-(4-chlorophenyl)-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(CN)C1=CC=C(Cl)C=C1 JYLNVJYYQQXNEK-UHFFFAOYSA-N 0.000 claims description 2
- VKJKEPKFPUWCAS-UHFFFAOYSA-M potassium chlorate Chemical compound [K+].[O-]Cl(=O)=O VKJKEPKFPUWCAS-UHFFFAOYSA-M 0.000 claims description 2
- 239000012286 potassium permanganate Substances 0.000 claims description 2
- 238000006555 catalytic reaction Methods 0.000 claims 3
- 239000007787 solid Substances 0.000 claims 3
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims 1
- 229910017604 nitric acid Inorganic materials 0.000 claims 1
- 229940001516 sodium nitrate Drugs 0.000 claims 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract description 13
- 239000000843 powder Substances 0.000 abstract description 4
- 229910002651 NO3 Inorganic materials 0.000 abstract description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000002245 particle Substances 0.000 description 5
- 239000013078 crystal Substances 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 2
- 229910021646 siderite Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910002588 FeOOH Inorganic materials 0.000 description 1
- 229910001035 Soft ferrite Inorganic materials 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- WJNPTRISSCIBDB-UHFFFAOYSA-N cobalt(2+) nickel(2+) tetranitrate Chemical compound [N+](=O)([O-])[O-].[Co+2].[Ni+2].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-] WJNPTRISSCIBDB-UHFFFAOYSA-N 0.000 description 1
- 150000001879 copper Chemical class 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000003670 easy-to-clean Effects 0.000 description 1
- 229960004887 ferric hydroxide Drugs 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- UCNNJGDEJXIUCC-UHFFFAOYSA-L hydroxy(oxo)iron;iron Chemical compound [Fe].O[Fe]=O.O[Fe]=O UCNNJGDEJXIUCC-UHFFFAOYSA-L 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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Abstract
本发明公开了一种固相催化氧化法生产α－Fe2O3的新方法，其技术关键是：以总铁含量≥71.2%铁矿粉或氧化铁皮为原料，经粉碎至150—325目，加入0.5—1.5%的锰酸盐类、高级锰钴镍氧化复合物、氯酸盐或硝酸盐类催化剂，在回转式氧化反应器中，于600—980℃下反应1—3.5h后经水洗、干燥、微粒化可制得α－Fe2O3，且α－Fe2O3的含量≥98.5%。本发明成本低廉，原料易得，工艺流程短，无污染，适于工业化生产。
The invention discloses a new method for producing α-Fe 2 O 3 by a solid-phase catalytic oxidation method. The technical key is: taking iron ore powder or iron oxide scale with a total iron content ≥ 71.2% as raw material, and crushing it to 150-325 mesh , add 0.5-1.5% of manganate, high-grade manganese-cobalt-nickel oxide complex, chlorate or nitrate catalyst, and react at 600-980°C for 1-3.5h in a rotary oxidation reactor. Washing, drying and micronization can produce α-Fe 2 O 3 , and the content of α-Fe 2 O 3 is ≥98.5%. The invention has low cost, easy-to-obtain raw materials, short process flow, no pollution and is suitable for industrialized production.
Description
本发明涉及一种α-Fe2O3的生产方法，特别是一种采用固相催化氧化法生产α-Fe2O3的新方法。The invention relates to a production method of α-Fe 2 O 3 , in particular to a new method for producing α-Fe 2 O 3 by adopting a solid-phase catalytic oxidation method.
高纯α-Fe2O3是制造软磁铁氧体的主要原料之一，在铁氧体配方中约占70％。软磁铁氧体在彩电、录像机、计算机、收录机、通讯设备等电子产品中有着极为广泛的用途，市场需求量很大。软磁铁氧体的性能对组分十分敏感，对原料α-Fe2O3的纯度、反应活性和晶体结构都有较高要求，若化学纯度较高，晶体结构良好，易于制造高档磁性器件，而且生产过程中工艺参数范围较宽，生产容易控制。α型三氧化二铁的生产工艺路线比较多，传统生产工艺一般分为干法和湿法两大类。传统湿法生产氧化铁红主要是以铁皮、铁屑为原料先制得亚铁盐，再加入碱液并通入空气，使其氧化生成Fe(OH)3，烘干即可制得Fe2O3，此法原料易得，但生成的Na2SO4不易处理，常大量加水冲稀而排放，造成环境污染，且Na2SO4的吸附能力较强，不易洗涤干净，影响产品质量，在生产过程中，空气量的多少、反应的PH值、温度及溶液的浓度等因素均影响产品的质量；干法生产是以硫酸亚铁、铁黄、铁黑或氢氧化铁及FeOOH等为原料，在高温下煅烧而制得Fe2O3，由于原料不同，工艺条件差异很大，干法生产工艺流程简单、投资较低，但废水、废气、粉尘污染均相当严重。High-purity α-Fe 2 O 3 is one of the main raw materials for making soft ferrite, accounting for about 70% in the ferrite formula. Soft magnetic ferrite is widely used in electronic products such as color TV sets, video recorders, computers, tape recorders, and communication equipment, and the market demand is very large. The performance of soft magnetic ferrite is very sensitive to the composition, and has high requirements on the purity, reactivity and crystal structure of the raw material α-Fe 2 O 3 . If the chemical purity is high and the crystal structure is good, it is easy to manufacture high-end magnetic devices. Moreover, the range of process parameters in the production process is wide, and the production is easy to control. There are many production process routes for α-type ferric oxide, and the traditional production processes are generally divided into two categories: dry process and wet process. The traditional wet method of production of iron oxide red mainly uses iron sheets and iron filings as raw materials to prepare ferrous salt first, then add lye and introduce air to oxidize it to form Fe(OH) 3 , and then dry it to obtain Fe 2 O 3. The raw materials of this method are easy to obtain, but the Na 2 SO 4 produced is not easy to handle. It is often diluted with a large amount of water and discharged, causing environmental pollution. Moreover, Na 2 SO 4 has a strong adsorption capacity and is not easy to clean, which affects product quality. In the production process, factors such as the amount of air, the pH value of the reaction, the temperature and the concentration of the solution all affect the quality of the product; dry production uses ferrous sulfate, iron yellow, iron black or ferric hydroxide and FeOOH as raw materials , Fe 2 O 3 is obtained by calcining at high temperature. Due to different raw materials, the process conditions vary greatly. The dry production process is simple and the investment is low, but the pollution of waste water, waste gas and dust is quite serious.
本发明的目的是提供一种以铁矿粉或氧化铁皮为原料，选用恰当的催化剂通过一步反应催化氧化法生产α-Fe2O3，以提高产品质量，缩短反应流程，降低产品成本，减少环境污染，克服现有技术的主要不足。The purpose of the present invention is to provide a method of producing α-Fe 2 O 3 by using iron ore powder or iron oxide scale as raw material and selecting an appropriate catalyst through a one-step reaction catalytic oxidation method, so as to improve product quality, shorten the reaction process, reduce product cost, and reduce environmental pollution and overcome the main shortcomings of the prior art.
下面详细叙述本发明的实现过程。Describe the realization process of the present invention in detail below.
附图1为本发明的工艺流程图。Accompanying drawing 1 is process flow diagram of the present invention.
如图所示，以总铁含量≥71.2％铁矿粉或氧化铁皮为原料，经粉碎至150-325目，加入0.5-1.5％的催化剂(锰酸盐类、高级锰钴镍氧化复合物，氯酸盐或硝酸盐类)，在不断通入空气，并同时通入约为空气量1-6％的水蒸气的回转式氧化反应器中，于氧化温度600-980℃下反应1-3.5h即可制得α-Fe2O3，再经水洗、干燥、微粒化可制得产品，α-Fe2O3的含量≥98.5％。As shown in the figure, the iron ore powder or iron oxide scale with a total iron content of ≥71.2% is used as raw material, crushed to 150-325 mesh, and 0.5-1.5% of catalyst (manganate, high-grade manganese-cobalt-nickel oxide compound, Chlorates or nitrates), in a rotary oxidation reactor that continuously feeds air and simultaneously feeds water vapor of about 1-6% of the air volume, reacts at an oxidation temperature of 600-980°C for 1-3.5 h to produce α-Fe 2 O 3 , and then washed with water, dried and micronized to obtain the product, the content of α-Fe 2 O 3 is ≥98.5%.
本发明所使用的催化剂锰酸盐类主要是锰酸钠、高锰酸钠、锰酸钾、高锰酸钾及伴有二氧化锰的混合物；氯酸盐为氯酸钠、氯酸钾；硝酸盐类是硝酸钠、硝酸钴硝酸镍及少量硝酸的铜盐；高级锰钴镍氧化复合物为MnO2·xNiO·yCoO(x,y=0.1-0.2)。反应使用回转式氧化反应器，如回转炉反应器，可使反应物充分接触，提高反应速度。在反应过程中通入约为空气量1-6％的水蒸气亦可促进氧化反应，方便操作。Catalyst manganate used in the present invention mainly is the mixture of sodium manganate, sodium permanganate, potassium manganate, potassium permanganate and manganese dioxide; Chlorate is sodium chlorate, potassium chlorate; Nitrate The class is sodium nitrate, cobalt nickel nitrate and a small amount of copper salt of nitrate; the advanced manganese cobalt nickel oxide complex is MnO 2 ·xNiO·yCoO(x,y=0.1-0.2). The reaction uses a rotary oxidation reactor, such as a rotary kiln reactor, which can fully contact the reactants and increase the reaction rate. The oxidation reaction can also be promoted by introducing water vapor of about 1-6% of the air volume during the reaction process, which is convenient for operation.
本发明的优点：通过铁矿粉或氧化铁皮一步法生产高纯α-Fe2O3成本比采用传统工艺低40％，原料易得，工艺流程短，无污染，催化剂易于洗脱，α-Fe2O3含量大于98.5％，适于工业化生产。The advantages of the present invention are: the cost of producing high-purity α-Fe 2 O 3 by one-step method of iron ore powder or iron oxide scale is 40% lower than that of the traditional process, the raw materials are easy to obtain, the process flow is short, no pollution, the catalyst is easy to elute, and α- The content of Fe 2 O 3 is greater than 98.5%, which is suitable for industrial production.
实施例1：以总铁含量大于71.2％的磁铁矿为原料，粉碎至粒度为325目，加入锰酸钠0.5％，不断通入空气，并同时通入约为空气量1-6％的水蒸气，750℃下在回转炉反应器中反应2h即可制得α-Fe2O3粗品，再经水洗、干燥、微粒化可制得产品。Embodiment 1: Using magnetite with a total iron content greater than 71.2% as raw material, pulverized to a particle size of 325 mesh, adding 0.5% sodium manganate, continuously feeding air, and simultaneously feeding about 1-6% of the air amount Steam, react in a rotary kiln reactor at 750°C for 2 hours to obtain the crude α-Fe 2 O 3 product, and then wash, dry, and micronize to obtain the product.
实施例2：以总铁含量大于71.2％的磁铁矿为原料，粉碎至粒度为200目，加入锰酸钾1.5％，不断通入空气，并同时通入约为空气量1-6％的水蒸气，850℃下在回转炉反应器中反应1h即可制得α-Fe2O3粗品，再经水洗、干燥、微粒化可制得产品。Embodiment 2: Using magnetite with a total iron content greater than 71.2% as raw material, pulverize to a particle size of 200 mesh, add 1.5% potassium manganate, continuously feed air, and simultaneously feed about 1-6% of the air amount Steam, react in a rotary kiln reactor at 850°C for 1 hour to obtain crude α-Fe 2 O 3 , and then wash, dry, and micronize to obtain the product.
实施例3：以总铁含量大于71.2％的菱铁矿为原料，粉碎至粒度为200目，加入锰钴镍氧化复合物0.8％，不断通入空气，并同时通入约为空气量1-6％的水蒸气，650℃下在回转炉反应器中反应1.5h即可制得α-Fe2O3粗品，再经水洗、干燥、微粒化可制得产品。Embodiment 3: Taking siderite with a total iron content greater than 71.2% as raw material, crushing to a particle size of 200 mesh, adding 0.8% of manganese-cobalt-nickel oxide compound, continuously feeding air, and simultaneously feeding about 1- 6% water vapor, react in a rotary kiln reactor at 650°C for 1.5h to produce crude α-Fe 2 O 3 , and then wash, dry, and micronize to obtain the product.
实施例4：以总铁含量大干71.2％的菱铁矿为原料，粉碎至粒度为200目，加入锰钴镍氧化复合物0.5％，不断通入空气，并同时通入约为空气量1-6％的水蒸气，850℃下在回转炉反应器中反应2.5h即可制得α-Fe2O3粗品，再经水洗、干燥、微粒化可制得产品。Embodiment 4: Taking siderite with a total iron content of up to 71.2% as raw material, pulverized to a particle size of 200 mesh, adding 0.5% of manganese-cobalt-nickel oxide compound, continuously feeding air, and simultaneously feeding about 1 -6% water vapor, react in a rotary kiln reactor at 850°C for 2.5 hours to obtain the crude α-Fe 2 O 3 product, and then wash, dry, and micronize to obtain the product.
实施例5：以总铁含量大于71.2％的氧化铁皮为原料，粉碎至粒度为150目，加入硝酸钠0.8％，不断通入空气，并同时通入约为空气量1-6％的水蒸气，700℃下在回转炉反应器中反应1.5h即可制得α-Fe2O3粗品，再经水洗、干燥、微粒化可制得产品。Example 5: Use iron oxide scale with a total iron content greater than 71.2% as raw material, crush it to a particle size of 150 mesh, add 0.8% sodium nitrate, continuously feed air, and simultaneously feed water vapor with an air volume of about 1-6% , α-Fe 2 O 3 crude product can be obtained by reacting in a rotary furnace reactor at 700°C for 1.5h, and then washed with water, dried and micronized to obtain the product.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2438616A (en) * | 2006-05-30 | 2007-12-05 | Iop Specialists Sdn Bhd | Iron oxide pigments from mill scale |
| CN102908896A (en) * | 2012-11-01 | 2013-02-06 | 昆明理工大学 | Method for catalytically oxidizing NO by dielectric barrier discharge plasma modified catalyst |
| 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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1998
- 1998-06-15 CN CN 98112890 patent/CN1239077A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2438616A (en) * | 2006-05-30 | 2007-12-05 | Iop Specialists Sdn Bhd | Iron oxide pigments from mill scale |
| GB2438616B (en) * | 2006-05-30 | 2011-01-05 | Iop Specialists Sdn Bhd | Iron oxide pigments from mill scale |
| CN102908896A (en) * | 2012-11-01 | 2013-02-06 | 昆明理工大学 | Method for catalytically oxidizing NO by dielectric barrier discharge plasma modified catalyst |
| CN102908896B (en) * | 2012-11-01 | 2015-07-22 | 昆明理工大学 | Method for catalytically oxidizing NO by dielectric barrier discharge plasma modified catalyst |
| 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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