CN1857775A - Carbonyl nickel powder and carbonyl iron powder on palygorskite carrier and their preparing method - Google Patents
Carbonyl nickel powder and carbonyl iron powder on palygorskite carrier and their preparing method Download PDFInfo
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- CN1857775A CN1857775A CN 200610051811 CN200610051811A CN1857775A CN 1857775 A CN1857775 A CN 1857775A CN 200610051811 CN200610051811 CN 200610051811 CN 200610051811 A CN200610051811 A CN 200610051811A CN 1857775 A CN1857775 A CN 1857775A
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- palygorskite
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 229910052625 palygorskite Inorganic materials 0.000 title claims abstract description 59
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims description 7
- 238000000197 pyrolysis Methods 0.000 claims abstract description 15
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 9
- 229910052742 iron Inorganic materials 0.000 claims abstract description 9
- 239000011707 mineral Substances 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 9
- 239000002245 particle Substances 0.000 claims abstract description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 238000005507 spraying Methods 0.000 claims description 7
- 239000012159 carrier gas Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 239000011777 magnesium Substances 0.000 claims description 3
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000391 magnesium silicate Substances 0.000 claims description 3
- 229910052919 magnesium silicate Inorganic materials 0.000 claims description 3
- 235000019792 magnesium silicate Nutrition 0.000 claims description 3
- 239000002923 metal particle Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims 1
- 238000000576 coating method Methods 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 14
- 229910052759 nickel Inorganic materials 0.000 abstract description 9
- 238000002360 preparation method Methods 0.000 abstract description 9
- 229910017147 Fe(CO)5 Inorganic materials 0.000 abstract description 6
- 238000004517 catalytic hydrocracking Methods 0.000 abstract description 6
- 238000005984 hydrogenation reaction Methods 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 4
- 229910052799 carbon Inorganic materials 0.000 abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 2
- 238000001704 evaporation Methods 0.000 abstract description 2
- 230000008020 evaporation Effects 0.000 abstract description 2
- 239000003208 petroleum Substances 0.000 abstract description 2
- 239000011148 porous material Substances 0.000 abstract description 2
- 230000002195 synergetic effect Effects 0.000 abstract description 2
- 238000009825 accumulation Methods 0.000 abstract 1
- 239000003513 alkali Substances 0.000 abstract 1
- 238000005137 deposition process Methods 0.000 abstract 1
- 230000002349 favourable effect Effects 0.000 abstract 1
- 238000001694 spray drying Methods 0.000 description 6
- 238000000746 purification Methods 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 239000000969 carrier Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000010779 crude oil Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000001376 precipitating effect Effects 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000004927 clay Substances 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229910019092 Mg-O Inorganic materials 0.000 description 1
- 229910019395 Mg—O Inorganic materials 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229960000892 attapulgite Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000013528 metallic particle Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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- Catalysts (AREA)
Abstract
The present invention discloses carbonyl nickel powder and carbonyl iron powder on palygorskite carrier. Palygorskite with intragranular tunnel pores can adsorb great amount of small molecular weight gas, such as H2, CO, CO2 and CH4, and is favorable to the synergistic effect of carbonyl nickel powder and carbonyl iron powder and can raise the catalytic efficiency. In addition, palygorskite is one kind of alkali mineral and can inhibit carbon accumulation during use to prolong the service life of the catalyst. The preparation process is one chemical evaporation and deposition process, and Ni(CO)4 or Fe(CO)5 vapor and palygorskite powder preheated to 180-300 deg.c are made to react inside a pyrolysis oven, so that the vapor is decomposed into fine Ni or Fe particles distributed homogeneously on the surface of palygorskite. The catalyst has high catalytic activity and long service life, and is used in petroleum hydrocracking and other hydrogenation reaction.
Description
Technical Field
The invention relates to carbonyl nickel powder and carbonyl iron powder taking palygorskite as a carrier and a preparation method thereof.
Background
The carbonyl nickel powder and the carbonyl iron powder are prepared from Ni (CO)4、Fe(CO)5The metal particles formed after the steam is decomposed by heating are catalysts for hydrocracking and hydrogenation reactions. Due to the shortage of light crude oil in international market, the crude oil of oil refining enterprises in China has become significantly heavy in recent years, and hydrocracking reaction is a main means for improving the utilization rate of crude oil and the yield of high-quality fuel oil. In addition, by the hydrogenation reaction, fuel or chemical raw material such as methane, methanol, formaldehyde and the like can be produced from carbon dioxide, and the CO can be reduced2Environmental problems caused by emission and simultaneously contributes to reasonable development and utilization of CO2And (4) resources. The nickel-based supported catalyst is widely applied due to low price and high catalytic activity. With the development of the hydrocracking and hydrogenation preparation fields, higher requirements are put on the performance of the nickel-based catalyst, especially the micronization of the carrier and nickel. The existing nickel-based and iron-based catalysts generally use artificially synthesized oxides, such as Al2O3、SiO2And ZrO2And the like, which are carriers of nickel, have defects such as poor bonding of the carrier to the metal fine particles, uneven distribution of the metal on the carrier, and the like to some extent, and the oxide fine particles used as the carrier are expensive. The development of novel catalysts and catalyst carriers is of great significance to the development of hydrocracking and hydrogenation preparation industries.
Disclosure of Invention
The invention aims to provide carbonyl nickel powder and carbonyl iron powder taking palygorskite as a carrier and a preparation method thereof.
The carbonyl nickel powder and carbonyl iron powder with palygorskite as carrier features that the palygorskite has nickel or iron particles adhered to its surface.
The palygorskite is a magnesium silicate mineral with a layer chain structure, and the theoretical molecular formula of the palygorskite is as follows:
Mg5Si8O20(OH)2(OH2)4·4H2O
the output form of the mineral is clay, mudstone, shale or loose blocky ore in nature. The carbonyl nickel powder or carbonyl iron powder is prepared from Ni (CO)4Or Fe (CO)5The steam is heated to decompose and form metal particles.
The preparation method of carbonyl nickel powder and carbonyl iron powder with palygorskite as a carrier comprises the following steps:
mixing Ni (CO)4Or Fe (CO)5Introducing steam into a closed cylindrical pyrolysis furnace, wherein the temperature in the pyrolysis furnace is 80-150 ℃, separating, purifying, spraying and drying the palygorskite powder, preheating to 180-300 ℃, spraying into the pyrolysis furnace under the carrying of nitrogen carrier gas, and introducing Ni (CO)4Or Fe (CO)5Steam is decomposed and deposited on the surface of the palygorskiteAnd precipitating to form carbonyl nickel powder and carbonyl iron powder, and attaching the carbonyl nickel powder and the carbonyl iron powder to the surface of the palygorskite to obtain the products, namely the carbonyl nickel powder and the carbonyl iron powder which take the palygorskite as a carrier.
The invention adopts natural palygorskite as the carrier of carbonyl nickel powder and carbonyl iron powder, and has the characteristics of wide source and low cost. The paligorskite crystal lattice is filled with tunnel holes and can adsorb a large amount of small molecule gas such as H2、CO、CO2And CH4The catalyst is beneficial to forming a synergistic effect with the carbonyl nickel powder and the carbonyl iron powder and improving the catalytic efficiency of the carbonyl nickel powder and the carbonyl iron powder. In addition, the palygorskite is an alkaline mineral, and can inhibit the formation of carbon deposit in the using process, thereby prolonging the service life of the catalyst. In the preparation method, the chemical evaporation precipitation method, namely the CVD method, is adopted to respectively mix Ni (CO)4、Fe(CO)5Reacting steam and palygorskite powder preheated to 180-300 ℃ in a pyrolysis furnace, wherein the reaction is Ni (CO)4、Fe(CO)5The steam is decomposed into metallic nickel and iron particles on the surface of the palygorskite, and the metallic particles are uniformly distributed on the carrier and are firmly combined with the carrier, so that the service life and the catalytic activity of the catalyst are longer than those of the traditional nickel-based and iron-based catalysts taking oxides as carriers.
The carbonyl nickel powder and carbonyl iron powder with palygorskite as carrier are suitable for hydrocracking petroleum and various hydrogenation reactions in chemical and chemical fields.
Detailed Description
Palygorskite is a natural magnesium silicate mineral with a chain-layered structure. The palygorskite is in a fibrous shape, the diameter of the palygorskite is 10-100 nanometers, the length of the palygorskite is several micrometers to dozens of micrometers, and in terms of single crystal size, the palygorskite accords with the definition of a nano material and belongs to typical natural one-dimensional nano minerals.
The theoretical molecular formula of palygorskite is:
Mg5Si8O20(OH)2(OH2)4·4H2O
on the crystal structure, a Mg-O (OH) octahedral layer is sandwiched between every two Si-O tetrahedral layers to form basic structural units, and the basic structural units are staggered to form a tunnel hole parallel to the lattice direction, and the cross section of the tunnel hole is 0.37 multiplied by 0.64 nanometers. The nano-sized intragranular tunnel pores enable the palygorskite to have huge specific surface area and adsorption-catalytic activity, which is the basis for being suitablefor serving as a catalyst carrier.
Palygorskite is commonly symbiotic with impurity minerals in nature, and tightly agglomerated with each other to produce clay, mudstone, shale or loose massive ore. The present invention uses the known technology to separate and purify natural palygorskite (also called attapulgite), and comprises the steps of crushing, pulping to prepare suspension, grading and collecting particles smaller than 5 mu, and spray drying. Wherein the purpose of the spray drying is to prevent agglomeration of the palygorskite during the dehydration process. The palygorskite after separation, purification and spray drying is one kind of loose powder with loose structure and loose mineral monocrystal contact, and is suitable for use as catalyst carrier. The separation and purification and spray drying process of the palygorskite can adopt conventional equipment.
The precursors of the carbonyl nickel powder and the carbonyl iron powder are respectively Ni (CO)4、Fe(CO)5Their preparation equipment and techniques are well known. Nickel tetracarbonyl and iron pentacarbonyl are easy to oxidize and need to be stored in an air-isolated manner before use.Ni(CO)4Boiling point 43 ℃, Fe (CO)5They have a boiling point of 103 ℃ and when heated to about 180 ℃ will immediately decompose into metallic nickel and metallic iron:
both of the above two formulae are endothermic reactions.
Firstly, Ni (CO)4Or Fe (CO)5Introducing steam into a closed cylindrical pyrolysis furnace, wherein the temperature in the furnace body is kept at 80-150 ℃; preheating the palygorskite powder subjected to separation and purification and spray drying to 180-300 ℃, spraying the palygorskite powder into a pyrolysis furnace under the carrying of nitrogen carrier gas, and carrying Ni (CO)4、Fe(CO)5And decomposing and precipitating the steam on the surface of the high-temperature palygorskite to form carbonyl nickel powder and carbonyl iron powder, and attaching the carbonyl nickel powder and the carbonyl iron powder to the surface of the palygorskite to obtain products, namely the carbonyl nickel powder and the carbonyl iron powder which take the palygorskite as a carrier. The product is precipitated at the bottom of the pyrolysis furnace and can be collected by a cloth bag, and CO is taken away by carrier gas.
The invention is further illustrated below with reference to specific examples.
Example 1:
mixing Ni (CO)4Introducing steam into a sealed 80 deg.C cylindrical pyrolysis furnace, preheating the spray-dried palygorskite powder to 180 deg.C, spraying into the pyrolysis furnace under the carrying of nitrogen carrier gas, and introducing into Ni (CO)4And decomposing and precipitating the steam on the surface of the palygorskite to form carbonyl nickel powder and attaching the carbonyl nickel powder to the surface of the palygorskite, wherein the obtained product is the carbonyl nickel powder taking the palygorskite as a carrier.
Example 2:
mixing Fe (CO)5Introducing steam into a sealed cylindrical pyrolysis furnace at 150 deg.C, preheating the palygorskite powder after separation and purification and spray drying to 300 deg.C, spraying into the pyrolysis furnace under the carrying of nitrogen carrier gas, and adding Fe (CO)5The steam is decomposed and precipitated on the surface of the palygorskite to form carbonyl iron powder which is attached to the surface of the palygorskite, and the obtained product is the carbonyl iron powder taking the palygorskite as a carrier.
Claims (4)
1. Carbonyl nickel powder and carbonyl iron powder with palygorskite as carrier features that the fine metallic nickel or iron particles are attached to the surface of palygorskite.
2. The carbonyl nickel powder and carbonyl iron powder on palygorskite carrier according to claim 1, wherein the palygorskite is a magnesium silicate mineral with a layer chain structure, and the theoretical formula of the palygorskite is as follows:
Mg5Si8O20(OH)2(OH2)4·4H2O
3. the carbonyl nickel powder or carbonyl iron powder on palygorskite carrier of claim 1, wherein the carbonyl nickel powder or carbonyl iron powder is composed of Ni (CO)4Or Fe (CO)5The steam is heated to decompose and form metal particles.
4. A method for preparing carbonyl nickel powder and carbonyl iron powder by using palygorskite as a carrier is characterized by comprising the following steps:
mixing Ni (CO)4Or Fe (CO)5Introducing steam into a closed cylindrical pyrolysis furnace, wherein the temperature in the pyrolysis furnace is 80-150 ℃, separating, purifying, spraying and drying the palygorskite powder, preheating to 180-300 ℃, spraying into the pyrolysis furnace under the carrying of nitrogen carrier gas, and introducing Ni (CO)4Or Fe (CO)5The steam is decomposed and precipitated on the surface of the palygorskite to form carbonyl nickel powder or carbonyl iron powder which is attached to the carbonyl nickel powder or the carbonyl iron powderAnd coating on the surface of the palygorskite to obtain the product, namely the carbonyl nickel powder or the carbonyl iron powder taking the palygorskite as a carrier.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610051811 CN1857775A (en) | 2006-06-05 | 2006-06-05 | Carbonyl nickel powder and carbonyl iron powder on palygorskite carrier and their preparing method |
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| CN 200610051811 CN1857775A (en) | 2006-06-05 | 2006-06-05 | Carbonyl nickel powder and carbonyl iron powder on palygorskite carrier and their preparing method |
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| CN101099932B (en) * | 2007-05-23 | 2010-04-21 | 江苏天一超细金属粉末有限公司 | High-efficient iron-series catalyst and its preparation method |
| US7897801B2 (en) | 2003-05-12 | 2011-03-01 | Invista North America S.A R.L. | Process for the preparation of dinitriles |
| US7919646B2 (en) | 2006-07-14 | 2011-04-05 | Invista North America S.A R.L. | Hydrocyanation of 2-pentenenitrile |
| US7973174B2 (en) | 2005-10-18 | 2011-07-05 | Invista North America S.A.R.L. | Process of making 3-aminopentanenitrile |
| US7977502B2 (en) | 2008-01-15 | 2011-07-12 | Invista North America S.A R.L. | Process for making and refining 3-pentenenitrile, and for refining 2-methyl-3-butenenitrile |
| US8088943B2 (en) | 2008-01-15 | 2012-01-03 | Invista North America S.A R.L. | Hydrocyanation of pentenenitriles |
| US8101790B2 (en) | 2007-06-13 | 2012-01-24 | Invista North America S.A.R.L. | Process for improving adiponitrile quality |
| US8178711B2 (en) | 2006-03-17 | 2012-05-15 | Invista North America S.A R.L. | Method for the purification of triorganophosphites by treatment with a basic additive |
| US8247621B2 (en) | 2008-10-14 | 2012-08-21 | Invista North America S.A.R.L. | Process for making 2-secondary-alkyl-4,5-di-(normal-alkyl)phenols |
| US8338636B2 (en) | 2009-08-07 | 2012-12-25 | Invista North America S.A R.L. | Hydrogenation and esterification to form diesters |
| US8373001B2 (en) | 2003-02-10 | 2013-02-12 | Invista North America S.A R.L. | Method of producing dinitrile compounds |
| US8906334B2 (en) | 2007-05-14 | 2014-12-09 | Invista North America S.A R.L. | High efficiency reactor and process |
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| US8373001B2 (en) | 2003-02-10 | 2013-02-12 | Invista North America S.A R.L. | Method of producing dinitrile compounds |
| US7897801B2 (en) | 2003-05-12 | 2011-03-01 | Invista North America S.A R.L. | Process for the preparation of dinitriles |
| US7973174B2 (en) | 2005-10-18 | 2011-07-05 | Invista North America S.A.R.L. | Process of making 3-aminopentanenitrile |
| US8178711B2 (en) | 2006-03-17 | 2012-05-15 | Invista North America S.A R.L. | Method for the purification of triorganophosphites by treatment with a basic additive |
| US7919646B2 (en) | 2006-07-14 | 2011-04-05 | Invista North America S.A R.L. | Hydrocyanation of 2-pentenenitrile |
| US8394981B2 (en) | 2006-07-14 | 2013-03-12 | Invista North America S.A R.L. | Hydrocyanation of 2-pentenenitrile |
| US8906334B2 (en) | 2007-05-14 | 2014-12-09 | Invista North America S.A R.L. | High efficiency reactor and process |
| CN101099932B (en) * | 2007-05-23 | 2010-04-21 | 江苏天一超细金属粉末有限公司 | High-efficient iron-series catalyst and its preparation method |
| US8101790B2 (en) | 2007-06-13 | 2012-01-24 | Invista North America S.A.R.L. | Process for improving adiponitrile quality |
| US7977502B2 (en) | 2008-01-15 | 2011-07-12 | Invista North America S.A R.L. | Process for making and refining 3-pentenenitrile, and for refining 2-methyl-3-butenenitrile |
| US8088943B2 (en) | 2008-01-15 | 2012-01-03 | Invista North America S.A R.L. | Hydrocyanation of pentenenitriles |
| US8247621B2 (en) | 2008-10-14 | 2012-08-21 | Invista North America S.A.R.L. | Process for making 2-secondary-alkyl-4,5-di-(normal-alkyl)phenols |
| US8338636B2 (en) | 2009-08-07 | 2012-12-25 | Invista North America S.A R.L. | Hydrogenation and esterification to form diesters |
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