CN107008339B - Organic sulfur non-hydroconversion catalyst and preparation method thereof - Google Patents

Organic sulfur non-hydroconversion catalyst and preparation method thereof Download PDF

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CN107008339B
CN107008339B CN201710284273.7A CN201710284273A CN107008339B CN 107008339 B CN107008339 B CN 107008339B CN 201710284273 A CN201710284273 A CN 201710284273A CN 107008339 B CN107008339 B CN 107008339B
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catalyst
organic sulfur
hydroconversion catalyst
hydroconversion
rare earth
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CN107008339A (en
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黄家鹄
黄晓榕
穆春雷
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SICHUAN HONGHU SCIENCE AND TECHNOLOGY GROUP Co Ltd
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SICHUAN HONGHU SCIENCE AND TECHNOLOGY GROUP Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/889—Manganese, technetium or rhenium
    • B01J23/8898—Manganese, technetium or rhenium containing also molybdenum
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/002—Mixed oxides other than spinels, e.g. perovskite
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
    • C10L3/06—Natural gas; Synthetic natural gas obtained by processes not covered by C10G, C10K3/02 or C10K3/04
    • C10L3/10—Working-up natural gas or synthetic natural gas
    • C10L3/101—Removal of contaminants
    • C10L3/102—Removal of contaminants of acid contaminants
    • C10L3/103—Sulfur containing contaminants
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2523/00—Constitutive chemical elements of heterogeneous catalysts

Abstract

The invention discloses an organic sulfur non-hydroconversion catalyst and a preparation method thereof, relating to the technical field of desulfurizing agents. The organic sulfur non-hydroconversion catalyst comprises a main agent and an auxiliary agent, wherein the main agent is selected from at least one of MnO2 and CuO and at least one of ZnO and Fe2O3, and the auxiliary agent is selected from at least one of rare earth and MoO 3. The formula of the catalyst has the effect of non-hydrogenation catalytic conversion, a hydrogenation conversion groove is not required to be arranged, hydrogen is not required to be supplemented in raw material gas, the process is short, the process cost is saved, and the conversion rate in the catalytic process is very high. The catalyst prepared by the method can realize non-hydrogenation catalytic conversion of high-concentration organic sulfur into H2S.

Description

Organic sulfur non-hydroconversion catalyst and preparation method thereof
Technical Field
The invention relates to the technical field of desulfurizing agents, and in particular relates to an organic sulfur non-hydroconversion catalyst and a preparation method thereof.
Background
At present, the catalytic conversion (absorption) method for organic sulfur in gaseous hydrocarbons (natural gas, oilfield associated gas and the like) mainly has the double functions of hydrolysis, catalytic hydrogenation conversion and catalytic hydrogenation conversion absorption.
The hydrolysis method mainly has conversion effect on the organic sulfur COS, can convert a small amount of CS2, and has no conversion function on other organic sulfur. The hydroconversion catalyst requires hydrogen for the conversion of organic sulfur; the gaseous hydrocarbon does not contain hydrogen, and the organic sulfur hydrogenation catalytic conversion can be realized only by supplementing hydrogen into the gaseous hydrocarbon. The dual-function desulfurizing agent for conversion and absorption of organic sulfur can replace both organic sulfur hydrogenation catalyst and zinc oxide desulfurizing agent, but it needs hydrogen gas.
Disclosure of Invention
The invention aims to provide an organic sulfur non-hydroconversion catalyst, which can realize non-hydroconversion and effectively remove high-concentration organic sulfur.
The invention also aims to provide a preparation method of the organic sulfur non-hydroconversion catalyst, the prepared catalyst has the function of non-hydroconversion and has high conversion rate in the process of catalytically removing the organic sulfur.
the technical problem to be solved by the invention is realized by adopting the following technical scheme.
The invention provides an organic sulfur non-hydroconversion catalyst, which comprises a main agent and an auxiliary agent, wherein the main agent is selected from at least one of MnO2 and CuO and at least one of ZnO and Fe2O3, and the auxiliary agent is selected from at least one of rare earth and MoO 3.
The invention also provides a preparation method of the organic sulfur non-hydroconversion catalyst, which comprises the steps of uniformly mixing the main agent, the auxiliary agent and the filler, molding, and roasting.
The organic sulfur non-hydroconversion catalyst and the preparation method thereof provided by the embodiment of the invention have the beneficial effects that: the catalyst formula of the invention comprises a main agent and an auxiliary agent, wherein the main agent is selected from at least one of MnO2 and CuO and at least one of ZnO and Fe2O3, the catalyst formula has the function of non-hydrogenation catalytic conversion, hydrogen does not need to be supplemented in raw material gas, and the conversion rate of organic sulfur in the catalytic process is very high. The catalyst prepared by the preparation method of the organic sulfur non-hydrogenation conversion catalyst provided by the invention can realize non-hydrogenation catalytic conversion and effectively remove high-concentration organic sulfur.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The organic sulfur non-hydroconversion catalyst and the preparation method thereof provided by the embodiments of the present invention are specifically described below.
the embodiment of the invention provides an organic sulfur non-hydroconversion catalyst, which comprises a main agent and an auxiliary agent, wherein the main agent is selected from at least one of MnO2 and CuO and at least one of ZnO and Fe2O3, and the auxiliary agent is selected from at least one of rare earth or MoO 3.
Particularly, CuO is a high-efficiency organic synthesis catalyst and can be used as a desulfurizer of oils to remove organic sulfur contained in the oils. ZnO can be used as a remover of H2S. MnO2 is a black amorphous powder that is commonly used as a sulfide (containing organic sulfur) remover, as an oxidant in organic chemistry, and also as a catalyst, especially as a denitration catalyst. Fe2O3 is reddish brown powder with metallic luster, is commonly used as a desulfurizing agent, and can also be used as a magnetic material, a pigment, a catalyst and the like. However, the main component of the formulation of the present invention is not always a commonly used desulfurizing agent.
Specifically, at least one of MnO2 and CuO and at least one of ZnO and Fe2O3 are selected as main agents in the formula of the catalyst, and at least one of rare earth and MoO3 is adopted as an auxiliary agent, so that the synergistic effect is realized through mutual cooperation, and the conversion rate of the formula of the catalyst in the process of catalytically removing organic sulfur is improved. In addition, the formula can realize the function of non-hydrogenation catalytic conversion and can adapt to different process requirements.
The organic sulfur non-hydroconversion catalyst further comprises a filler, wherein the filler is at least one selected from kaolin, diatomite, alumina, graphite and carbon black. The filler is added into the formula of the catalyst, so that the effects of capacity increase and weight increase can be achieved, the contact area of the catalyst and organic matters can be increased, and the desulfurization effect of the catalyst can be improved.
Further, the organic sulfur non-hydroconversion catalyst comprises the following components in percentage by mass: MnO 28-35%, Fe2O 35-42%, CuO 1-40%, ZnO 2-35%, rare earth 0.2-2%, MoO30.3-2%, and filler 1-30%. The dosage of the main agent and the auxiliary agent in the catalyst formula is controlled within the range, the catalyst has the function of non-hydrogenation catalytic conversion, can improve the desulfurization rate of the catalyst formula, and is particularly suitable for organic sulfur conversion in gaseous hydrocarbon containing high-concentration organic sulfur and no hydrogen, such as natural gas, oil field gas and the like. The catalyst can be matched with NHD (polyethylene glycol dimethyl ether), Sulfinol solvent and a temperature swing adsorption method to be used as an organic sulfur conversion catalyst in regenerated waste gas.
It is noted that when the organic sulfur content is up to 5000-. The catalyst does not need to be presulfided in advance before use, and the new catalyst has both an organic non-hydrogenation catalytic conversion function and an H2S absorption function at the beginning of use. As the metal oxide in the catalyst is converted to a metal sulfide, the catalyst still has catalytic activity but no longer has H2S absorption function.
Preferably, the organosulfur non-hydroconversion catalyst comprises, in mass fractions: 225-28% of MnO, 323-28% of Fe2O, 15-25% of CuO, 15-25% of ZnO, 0.2-2% of rare earth, 30.3-2% of MoO30 and 2-20% of filler. The contents of the main agent, the auxiliary agent and the filler in the catalyst formula are accurately controlled within a certain range, so that the catalytic activity of the catalyst formula can be effectively maintained. The preferred ranges for each component in the catalyst formulation are obtained through multiple laboratory pilot plant and engineering practices.
Further, MnO2 is prepared by decomposing MnCO3, and Fe2O3 is prepared by decomposing Fe (OH) 3. MnO2 is prepared by thermal decomposition reaction of MnCO3 under oxygen-free condition, and Fe2O3 is prepared by thermal decomposition of Fe (OH) 3. Specifically, MnO2 and Fe2O3 can be selectively prepared or purchased according to the stock conditions of the raw materials, so that the production cost is reduced.
Further, MoO3 in the auxiliary agent is prepared from industrial ammonium molybdate, and the rare earth in the auxiliary agent is industrial product rare earth metal oxide. The MoO3 is prepared by adopting an industrial ammonium molybdate thermal dissociation mode, the cost of the catalyst formula can be reduced, and the MoO3 prepared by performing thermal dissociation on ammonium molybdate has high purity and can completely meet the requirement of the catalyst. The rare earth metal oxide has high chemical activity, luster between silver and iron, and good cohesiveness, expansibility and adsorbability. The rare earth metal is used as an auxiliary agent, so that the dispersing performance of the catalyst and the absorbing capacity of H2S can be obviously improved.
It should be noted that, taking methyl mercaptan as an example, the catalytic principle of the organic sulfur non-hydroconversion catalyst provided by the present invention is specifically described. The reaction equation for a conventional hydrocatalytic process is: CH3SH + H2 ═ CH4+ H2S, the reaction equation for the catalytic process of the non-hydroconversion catalyst is: 2CH3SH ═ C2H4+2H2S, the organic sulfur non-hydroconversion catalyst provided by the invention can convert organic sulfur into unsaturated hydrocarbon and hydrogen sulfide under the reaction condition without hydrogen, and saturated hydrocarbon is generated in the process of hydrocatalytic conversion. The organic sulfur non-hydrogenation conversion catalyst provided by the invention can realize a non-hydrogenation process, a multi-stage hydrogenation conversion tank is not required to be arranged in the catalytic conversion process, the process is relatively shorter, the cost is low, and the catalyst has an H2S absorption function, so that the process cost of subsequent treatment is reduced.
The embodiment of the invention also provides a preparation method of the organic sulfur non-hydroconversion catalyst, which comprises the steps of uniformly mixing the main agent, the auxiliary agent and the filler, forming, and then roasting.
Specifically, the main agent, the auxiliary agent and the filler in the formula are weighed according to the formula proportion, are uniformly mixed by adopting a mechanical stirring mode and the like, are prepared into the catalyst with a specific shape according to the process requirement, and are roasted at the temperature of 350 ℃ below 300 ℃ to remove water and ensure that the catalyst is more uniformly attached to the surface of the carrier, so that the loss of the catalyst along with the solution is prevented.
Specifically, the forming process adopts any one of dry-mixing extrusion molding, rolling ball molding or pressing molding. The dry-mixed extrusion molding adopts a mode of not adding a fusing agent and is formed by a strip extruding machine. The extrusion molding, the rolling ball molding and the pressing molding are conventional technical means in the catalyst molding process.
The features and properties of the present invention are described in further detail below with reference to examples.
example 1
The embodiment provides an organic sulfur non-hydroconversion catalyst, which comprises the following components in percentage by mass: MnO 28%, Fe2O 342%, CuO 40%, ZnO 3%, rare earth 2%, MoO 32% and filler 3%.
The embodiment also provides a preparation method of the organic sulfur non-hydroconversion catalyst, which comprises the steps of uniformly mixing the raw materials in the catalyst formula, dry-mixing, extruding, molding and roasting at 300 ℃.
Example 2
The embodiment provides an organic sulfur non-hydroconversion catalyst, which comprises the following components in percentage by mass: MnO 235%, Fe2O 35%, CuO23.5%, ZnO 35%, rare earth 0.2%, MoO30.3% and filler 1%.
The embodiment also provides a preparation method of the organic sulfur non-hydroconversion catalyst, which comprises the steps of uniformly mixing the raw materials in the catalyst formula, dry-mixing, extruding, molding and roasting at 350 ℃.
Example 3
The embodiment provides an organic sulfur non-hydroconversion catalyst, which comprises the following components in percentage by mass: 215% of MnO, 342% of Fe2O, 1% of CuO, 8% of ZnO, 2% of rare earth, 32% of MoO and 30% of filler.
This example also provides a method for preparing a non-hydroconversion organosulfur catalyst, which comprises mixing the raw materials in the above catalyst formulation, rolling ball forming, and calcining at 325 ℃.
Example 4
The embodiment provides an organic sulfur non-hydroconversion catalyst, which comprises the following components in percentage by mass: MnO 225%, Fe2O334.1%, CuO 35%, ZnO 2%, rare earth 1.2%, MoO31.7% and filler 1%.
The embodiment also provides a preparation method of the organic sulfur non-hydroconversion catalyst, which comprises the steps of uniformly mixing the raw materials in the catalyst formula, dry-mixing, extruding, molding and roasting at 300 ℃.
Example 5
The embodiment provides an organic sulfur non-hydroconversion catalyst, which comprises the following components in percentage by mass: MnO 228%, Fe2O 323%, CuO 25%, ZnO18.5%, rare earth 2%, MoO31.5% and filler 2%.
The embodiment also provides a preparation method of the organic sulfur non-hydroconversion catalyst, which comprises the steps of uniformly mixing the raw materials in the catalyst formula, dry-mixing, extruding, molding and roasting at 300 ℃.
Example 6
The embodiment provides an organic sulfur non-hydroconversion catalyst, which comprises the following components in percentage by mass: MnO 228%, Fe2O 328%, CuO 18%, ZnO 20%, rare earth 2%, MoO 32% and filler 2%.
This example also provides a method for preparing a non-hydroconversion organosulfur catalyst, which comprises mixing the raw materials in the above catalyst formulation, rolling ball forming, and then calcining at 300 ℃.
Example 7
The embodiment provides an organic sulfur non-hydroconversion catalyst, which comprises the following components in percentage by mass: MnO 225%, Fe2O 323%, CuO 15%, ZnO 25%, rare earth 2%, MoO30.3% and filler 9.7%.
The embodiment also provides a preparation method of the organic sulfur non-hydroconversion catalyst, which comprises the steps of uniformly mixing the raw materials in the catalyst formula, dry-mixing, extruding, molding and roasting at 350 ℃.
Example 8
The embodiment provides an organic sulfur non-hydroconversion catalyst, which comprises the following components in percentage by mass: MnO226.5%, Fe2O 323%, CuO 15%, ZnO 15%, rare earth 0.2%, MoO30.3% and filler 20%.
The embodiment also provides a preparation method of the organic sulfur non-hydroconversion catalyst, which comprises the steps of uniformly mixing the raw materials in the formula of the catalyst, pressing and molding the mixture, and then roasting the mixture at 300 ℃.
Test examples
The organosulfur non-hydroconversion catalysts of examples 4-8 were tested for performance by the following methods:
(1) Sampling: the natural gas before and after non-hydrogenation catalytic conversion is analyzed, the organic sulfur content before the conversion is Xmg/Nm3, the organic sulfur content after the conversion is Ymg/Nm3, and X, Y is the content of sulfur elements in the organic sulfur in the natural gas. The organic sulfur mainly comprises methyl mercaptan, ethanethiol, methyl sulfide, methyl ethyl sulfide and the like, and cannot generate H2S through hydrolysis;
(2) And (3) catalytic conversion conditions: heating natural gas to 300-450 ℃ and then passing through a non-hydrogenation catalyst bed layer;
(3) An analytical instrument: flame photometric detection gas chromatography trace sulfur analyzer;
(4) Conversion calculation formula: conversion (%) - (X-Y)/X.
The desulfurization rate of the organic sulfur non-hydroconversion catalyst prepared in the example was determined by the above detection method, and was determined by a flame photometric detection gas chromatography trace sulfur analyzer. The desulfurization rates of the organosulfur non-hydroconversion catalysts of examples 4-8 were: 99.7, 99.9, 99.8, 99.9. Therefore, the catalyst prepared by combining the formula of the catalyst provided by the invention with the existing catalyst preparation method can effectively convert organic sulfur, and the conversion rate is as high as 99.9%. The conversion rate of the organic sulfur in the prior art can reach 99.7 percent only by two-stage hydrogenation, and the equipment cost is far higher than that of the organic sulfur non-hydrogenation conversion catalyst in the invention.
In summary, the organic sulfur non-hydroconversion catalyst provided by the invention adopts at least one of MnO2 and CuO and at least one of ZnO and Fe2O3 as main agents, and at least one of rare earth or MoO3 as auxiliary agents. The catalyst formula has high conversion rate in the process of catalytically removing organic sulfur, can realize the effect of non-hydrogenation catalytic conversion, has the function of absorbing H2S, and can adapt to different process requirements. The invention also provides a preparation method of the organic sulfur non-hydroconversion catalyst, which is characterized in that the raw materials in the formula are uniformly mixed, molded and roasted, and the prepared catalyst has the effect of non-hydroconversion and has the desulfurization rate of 99.9 percent.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Claims (9)

1. An organic sulfur non-hydroconversion catalyst, characterized in that,
The organic sulfur non-hydroconversion catalyst comprises the following components in percentage by mass: MnO 28-35%, Fe2O 35-42%, CuO 1-40%, ZnO 2-35%, rare earth 0.2-2%, MoO30.3-2%, and filler 1-30%.
2. The organosulfur non-hydroconversion catalyst of claim 1, wherein the filler is selected from at least one of kaolin, diatomaceous earth, alumina, graphite, and carbon black.
3. The organosulfur non-hydroconversion catalyst according to claim 1, comprising in mass fraction: 225-28% of MnO, 323-28% of Fe2O, 15-25% of CuO, 15-25% of ZnO, 0.2-2% of rare earth, 30.3-2% of MoO30 and 2-20% of filler.
4. The organosulfur non-hydroconversion catalyst of claim 3, wherein the MnO2 is prepared from decomposition of MnCO 3.
5. The organosulfur non-hydroconversion catalyst of claim 3, wherein the Fe2O3 is produced by decomposition of Fe (OH) 3.
6. The organosulfur non-hydroconversion catalyst of claim 3, wherein MoO3 is prepared from commercial ammonium molybdate.
7. the organosulfur non-hydroconversion catalyst of claim 3, wherein the rare earth is an industrial product rare earth metal oxide.
8. A method for preparing the organic sulfur non-hydroconversion catalyst according to any one of claims 1 to 7, comprising the steps of uniformly mixing raw materials of the organic sulfur non-hydroconversion catalyst, molding, and then roasting.
9. The method of claim 8, wherein the molding process is carried out by dry-blending extrusion molding or ball-rolling molding.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1047219A (en) * 1990-02-27 1990-11-28 黄家鹄 Remove the low-temp desulfurization agent of organosulfur in the gas
CN1813043A (en) * 2003-07-11 2006-08-02 阿斯彭产品集团公司 Methods and compositions for desulfurization of hydrocarbon fuels

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CN100341983C (en) * 2005-04-19 2007-10-10 湖北省化学研究院 Converting and absorbing fine desulfurizer and its prepn

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1047219A (en) * 1990-02-27 1990-11-28 黄家鹄 Remove the low-temp desulfurization agent of organosulfur in the gas
CN1813043A (en) * 2003-07-11 2006-08-02 阿斯彭产品集团公司 Methods and compositions for desulfurization of hydrocarbon fuels

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