CN106311339A - Catalyst used for coal hydrogenation catalytic gasification, and preparation method and use thereof - Google Patents
Catalyst used for coal hydrogenation catalytic gasification, and preparation method and use thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of coal hydrogenation catalytic gasification catalysts, and provides a high-efficiency catalyst used for coal hydrogenation catalytic gasification, and a preparation method thereof. The above ternary composite catalyst is obtained through depositing a ternary active component of the catalyst on a coal-based material by adopting a simple and effective precipitation technology, and surface function groups on the coal-based material have strong interaction with the catalyst components. Compared with a unitary component and a binary component, the ternary component applied in the reaction for preparing natural gas through coal hydrogenation catalytic gasification has a low melting point, easily becomes a liquid rapidly penetrating apertures in the coal-based material in order to improve the gasification efficiency of the coal, can be easily combined with the coal in the presence of organic potassium or sodium salt, and generates a large amount of apertures in the high temperature reaction process. A result of active test shows that the prepared Fe-Ca-Na catalyst allows the rate of conversion of the coal into a gaseous product to reach 75.2% and the methane generation amount to be 3.7 mmol.g<-1> when the reaction time is 300 min.
Description
Technical field
The invention belongs to catalysis technical field, relate to a kind of efficient for coal hydrogenation catalytic gasification catalyst and preparation method thereof.
Background technology
The utilization of coal in China is based on direct burning, and not only energy utilization rate is the lowest, and causes dust, acid rain, a large amount of greenhouse gases CO2The pollution problems such as discharge, Coal Gasification Technology plays an important role in terms of efficient, clean utilization coal resources, but traditional coal gasification course reaction temperature is high, generates gas and purifies difficulty, and energy consumption is big, high to equipment requirements.
The various new type coal gasification technology being in the laboratory research stage are referred to as third generation Coal Gasification Technology, including the catalytic gasification technology of coal.Conventional natural gas from coal technology (two-step method) is to convert coal into synthesis gas under the conditions of high temperature (800-1500 DEG C) and certain pressure (2-4MPa), synthesis gas obtains substituting natural gas again after methanation, this technical process comparative maturity, but technological process is long, investment is big, and process thermal efficiency is low.Coal direct hydrogenation vaporizing system natural gas technology is under the conditions of uniform temperature (800-1000 DEG C) and certain pressure (3-10MPa), fine coal and hydrogen are simultaneously introduced gasification furnace, rely on hydrogen that the pyrolysis of coal stage release Stabilization of free radical and gasifying stage and the reaction of the carbon of activity in semicoke obtain the gas of methane rich, simultaneously the liquid organic products such as BTX and PCX of by-product high added value.Compared with two-step method, this technological process is simple, and low and process the thermal efficiency of cost of investment is higher, reduces the requirement to gasification furnace equipment and materials, and the beneficially desulfurization of gasification, dedusting.Therefore, coal hydrogenation catalytic gasification technology is increasingly paid attention to by domestic and international researcher.
Substantial amounts of result of study shows alkali metal compound especially potassium, the carbonate of sodium, and the salt of alkaline-earth metal and transition metal is all the good catalyst of catalytic gasification.Exxonmobil company of the U.S. is with K2CO3As catalyst, have developed the pressurised fluidized bed catalysis gasification technique of the coal for the purpose of producing substitute natural gas, add K2CO3After catalyst, within the same reaction time, efficiency of carbon con version is greatly improved, and reaction rate also improves about 4 times of (Energy
Research,1980,4:137-147).Compared with single component catalyst, multicomponent catalyst has higher gasification efficiency, is recently paid high attention to by researcher.Akyurtlu etc. are with K2SO4And FeSO4Mixture be that catalyst carries out gasification research to Pittsburgh's HVA coal tar, reaction condition is: K/Fe mol ratio is 9, temperature is 850 DEG C, pressure is 0.1MPa, the atomic ratio of metal/carbon is 0.02, content of metal is 5.1～7.3g/100g carbon, carbon granule size is 53 μm～106 μm, reaction gas are H2O/H2Or H2O/N2(H2O content is 30%), charcoal percent conversion can reach 100%, under same reaction conditions, is used alone K2CO3As catalyst, charcoal percent conversion is only 89%(Fuel Processing Technology, and 1995,43:71-86).Sheth etc. use three-way catalyst Li respectively2CO3-Na2CO3-K2CO3, binary catalyst Na2CO3-K2CO3, monolithic catalyst K2CO3Coal is carried out gasification kinetics research, find that the activation energy of catalytic gasification is less than binary catalyst and the activation energy of monolithic catalyst catalytic gasification, this is owing to, under gasification temperature (700 DEG C～900 DEG C), three-way catalyst is in a liquid state, and binary catalyst and monolithic catalyst K2CO3For solid-state.Owing to catalyst exists with liquid, its good fluidity, it is easier to be diffused into reaction system, the active sites of coal increases accordingly, the most active of a relatively high (Fuel, 2004,83:557-572).But, in gasification, base metal catalysts is easily made catalyst action weaken by mineral passivation, and methanation productivity is low.Therefore, being badly in need of exploitation one not easy in inactivation, methanation is effective, can be used for coal hydrogenation catalytic gasification catalyst, it is achieved catalytic coal gasifaction technology industrialization bottleneck is broken through.
Summary of the invention
Object of the present invention is to provide a kind of efficient for coal hydrogenation catalytic gasification catalyst and preparation method thereof.
Technical scheme: a kind of for coal hydrogenation catalytic gasification catalyst and preparation method thereof, it is characterized in that described catalyst comprises component A, B component, component C and coal sill, metal species in component A mass fraction in the catalyst is 1%-5%, metal species in B component mass fraction in the catalyst is 1%-5%, metal species in component C mass fraction in the catalyst is 1%-15%, remaining composition is mainly coal sill, and particle diameter is 40 mesh-80 mesh.
Described component A is one or more in nickel salt and iron salt.
Described B component is one or more in the calcium salt of solubility, magnesium salt, manganese salt and zinc salt.
Described component C is one or more in Organic Sodium Salt and potassium salt.
The one of which or several such as described component C preferably sodium dodecyl sulfate, enuatrol, potassium oleate and polyacrylamide potassium salt.
The mixing of component A, B component, component C and coal sill is placed in water by the preparation method of described catalyst: a., stirs；B. the mixture that step a prepares is added in autoclave, carry out hydrothermal treatment consists；C. the material in autoclave is taken out, carry out washing, dried；The most dried material is pressed into tablet.
The described water preferred electrical conductivity water less than 5 μ s/cm.
Described method for preparing catalyst, it is characterised in that hydrothermal treatment consists is usually at 80 DEG C ~ 200 DEG C, and pressure is at 2.0MPa ~ 10.0MPa, and the time is 3h-5h.
Described catalyst is applied in the reaction of coal hydrogenation catalytic gasification preparing natural gas.
The significant advantage that the present invention is presented shows themselves in that
A. the present invention is under high temperature, condition of high voltage, three kinds of effective active components is deposited on carbon-based material with the sedimentation method, and High Temperature High Pressure can change biomass structure in coal base, promotes that coal sill is combined with catalyst.The organic potassium of component C the most of the present invention employing or sodium salt, organic salt is easier to close with coal base junction, produces a large amount of hole when pyroreaction, promote that reaction is carried out.C. in gasification reaction, compared with one pack system, ternary component has lower fusing point, easily being changed into liquid, it is possible in rapid osmotic to the hole of coal sill, catalyst effective ingredient is A simultaneously, promote methanation reaction, B component is that component C accelerates water gas shift reaction in order to absorb the acidic materials produced in gasification, improves H2Content, in order to react generation methane with carbon.Active testing result shows, under high temperature, condition of high voltage, when component C is organic salt, the three-way catalyst of preparation has higher coal and is changed into conversion ratio and the methane-generated quantity of gas-phase product.
Detailed description of the invention
Embodiment
1
By 0.25 g Ni (NO3)2、0.16 g Mn(Ac)2With 3.79 g C18H29NaO3S is dissolved in 40 ml deionized waters, then 5 g bituminous coal are joined in above-mentioned solution, be sufficiently stirred for making it mix, above-mentioned solution is joined in autoclave, at 3.5MP, 180 DEG C of hydrothermal treatment consists 5h, take out the material in autoclave, carry out washing, dried, it is pressed into tablet, grinding is sieved, and is labeled as Sample1, standby.On this catalyst, coal is changed into conversion ratio versus time curve and the CH of gas-phase product4Growing amount is shown in Table 1 respectively.
Embodiment
2
By 0.25 g Ni (NO3)2、0.16 g Mn(Ac)2With 3.48 g C18H33O2Na is dissolved in 40 ml deionized waters, then 5 g bituminous coal are joined in above-mentioned solution, be sufficiently stirred for making it mix, above-mentioned solution is joined in autoclave, at 3.5MP, 180 DEG C of hydrothermal treatment consists 5h, take out the material in autoclave, carry out washing, dried, it is pressed into tablet, grinding is sieved, and is labeled as Sample2, standby.On this catalyst, coal is changed into conversion ratio versus time curve and the CH of gas-phase product4Growing amount is shown in Table 1 respectively.
Embodiment
3
By 0.25g Ni (NO3)2、0.16g Mn(Ac)2With 3.28g C18H33O2K is dissolved in 40 ml deionized waters, then 5 g bituminous coal are joined in above-mentioned solution, be sufficiently stirred for making it mix, above-mentioned solution is joined in autoclave, at 3.5MP, 180 DEG C of hydrothermal treatment consists 5h, take out the material in autoclave, carry out washing, dried, it is pressed into tablet, grinding is sieved, and is labeled as Sample3, standby.On this catalyst, coal is changed into conversion ratio versus time curve and the CH of gas-phase product4Growing amount is shown in Table 1 respectively.
Embodiment
4
By 0.25 g Ni (NO3)2、0.09 g Ca(OH)2With 3.48 g C18H33O2Na is dissolved in 40 ml deionized waters, then 5 g bituminous coal are joined in above-mentioned solution, be sufficiently stirred for making it mix, above-mentioned solution is joined in autoclave, at 3.5MP, 180 DEG C of hydrothermal treatment consists 5h, take out the material in autoclave, carry out washing, dried, it is pressed into tablet, grinding is sieved, and is labeled as Sample4, standby.On this catalyst, coal is changed into conversion ratio versus time curve and the CH of gas-phase product4Growing amount is shown in Table 1 respectively.
Embodiment
5
By 0.25 g Ni (NO3)2、0.22 g Zn(NO3)2With 3.48g C18H33O2Na is dissolved in 40 ml deionized waters, then 5 g bituminous coal are joined in above-mentioned solution, be sufficiently stirred for making it mix, above-mentioned solution is joined in autoclave, at 3.5MP, 180 DEG C of hydrothermal treatment consists 5h, take out the material in autoclave, carry out washing, dried, it is pressed into tablet, grinding is sieved, and is labeled as Sample5, standby.On this catalyst, coal is changed into conversion ratio versus time curve and the CH of gas-phase product4Growing amount is shown in Table 1 respectively.
Embodiment
6
By 0.2 g NiCl2·6H2O、0.09g Ca(OH)2With 3.48 g C18H33O2Na is dissolved in 40 ml deionized waters, then 5 g bituminous coal are joined in above-mentioned solution, be sufficiently stirred for making it mix, above-mentioned solution is joined in autoclave, at 3.5MP, 180 DEG C of hydrothermal treatment consists 5h, take out the material in autoclave, carry out washing, dried, it is pressed into tablet, grinding is sieved, and is labeled as Sample6, standby.On this catalyst, coal is changed into conversion ratio versus time curve and the CH of gas-phase product4Growing amount is shown in Table 1 respectively.
Embodiment
7
By 0.28 g Fe2(SO4)3、0.09 g Ca(OH)2With 3.48 g C18H33O2Na is dissolved in 40 ml deionized waters, then 5 g bituminous coal are joined in above-mentioned solution, be sufficiently stirred for making it mix, above-mentioned solution is joined in autoclave, at 3.5MP, 180 DEG C of hydrothermal treatment consists 5h, take out the material in autoclave, carry out washing, dried, it is pressed into tablet, grinding is sieved, and is labeled as Sample7, standby.On this catalyst, coal is changed into conversion ratio versus time curve and the CH of gas-phase product4Growing amount is shown in Table 1 respectively.
Embodiment
8
By 0.24g FeCl3·6H2O、0.09g Ca(OH)2With 3.84 g C18H33O2Na is dissolved in 40 ml deionized waters, then 5 g bituminous coal are joined in above-mentioned solution, be sufficiently stirred for making it mix, above-mentioned solution is joined in autoclave, at 3.5MP, 180 DEG C of hydrothermal treatment consists 5h, take out the material in autoclave, carry out washing, dried, it is pressed into tablet, grinding is sieved, and is labeled as Sample8, standby.On this catalyst, coal is changed into conversion ratio versus time curve and the CH of gas-phase product4Growing amount is shown in Table 1 respectively.
Embodiment
9
By 0.24g FeCl3·6H2O、0.09g Ca(OH)2With 3.84 g C18H33O2Na is dissolved in 40 ml deionized waters, then 5 g bituminous coal are joined in above-mentioned solution, be sufficiently stirred for making it mix, above-mentioned solution is joined in autoclave, at 2MP, 80 DEG C of hydrothermal treatment consists 5h, take out the material in autoclave, carry out washing, dried, it is pressed into tablet, grinding is sieved, and is labeled as Sample9, standby.On this catalyst, coal is changed into conversion ratio versus time curve and the CH of gas-phase product4Growing amount is shown in Table 1 respectively.
Control experiment
By 0.24g FeCl3·6H2O、0.09g Ca(OH)2With 0.58 gNa2CO3It is dissolved in 40 ml deionized waters, then 5 g bituminous coal are joined in above-mentioned solution, be sufficiently stirred for making it mix, above-mentioned solution is joined in autoclave, at 3.5MP, 180 DEG C of hydrothermal treatment consists 5h, take out the material in autoclave, carry out washing, dried, it is pressed into tablet, grinding is sieved, and is labeled as Sample10, standby.On this catalyst, coal is changed into conversion ratio versus time curve and the CH of gas-phase product4Growing amount is shown in Table 1 respectively.
By 0.09g Ca (OH)2With 3.84 g C18H33O2Na is dissolved in 40 ml deionized waters, then 5 g bituminous coal are joined in above-mentioned solution, be sufficiently stirred for making it mix, above-mentioned solution is joined in autoclave, at 3.5MP, 180 DEG C of hydrothermal treatment consists 5h, take out the material in autoclave, carry out washing, dried, it is pressed into tablet, grinding is sieved, and is labeled as Sample11, standby.On this catalyst, coal is changed into conversion ratio versus time curve and the CH of gas-phase product4Growing amount is shown in Table 1 respectively.
By 3.84 g C18H33O2Na is dissolved in 40 ml deionized waters, then 5 g bituminous coal are joined in above-mentioned solution, be sufficiently stirred for making it mix, above-mentioned solution is joined in autoclave, at 3.5MP, 180 DEG C of hydrothermal treatment consists 5h, take out the material in autoclave, carry out washing, dried, it is pressed into tablet, grinding is sieved, and is labeled as Sample12, standby.On this catalyst, coal is changed into conversion ratio versus time curve and the CH of gas-phase product4Growing amount is shown in Table 1 respectively.
Catalyst performance evaluation
The evaluation of catalyst, at 700 DEG C, is carried out under 3.5MPa reaction system, and this system is to regulate pressure by Ar gas, and fixed bed reactors internal diameter is 32 mm, high 800 mm.The mixture of catalyst with coal dust (or coal tar), by heating up, boost temperature, the pressure reaching to set, is disposably pressed into reactor by forced feed pump by system, by precision metering pump, liquid phase water is squeezed into carburator, and the laggard reactor of water vapor starts reaction.Product gas enters knockout drum and carries out gas-liquid separation, the gas drying device dehumidifying after separation, after wet flow indicator measures, then is collected by airbag, eventually passes product gas composition and content that GC analyzes in every period.
Table
1
, in different time, coal is changed into conversion ratio and the methane accumulation growing amount of gas-phase product on catalyst
A coal is changed into the conversion ratio of gas-phase product。
B methane-generated quantity。
From table 1, in the reaction of catalytic coal gasifaction preparing natural gas, under same reaction process situation, organic potassium or sodium salt, organically salt is easier to close with coal base junction, a large amount of hole is produced when pyroreaction, , the coal of ternary complex catalyst is changed into the conversion ratio of gas-phase product and methane-generated quantity and is changed into conversion ratio and the methane-generated quantity of gas-phase product far above the coal on unitary catalyst and binary catalyst, wherein Sample8 is when reaction proceeds to 300 minutes, on this catalyst, coal is changed into the conversion ratio of gas-phase product and reaches 75.2%, wherein the growing amount of methane is 3.7 mmol
g-1, demonstrate the methane performance processed of excellence.
Claims (9)
1. one kind is used for coal hydrogenation catalytic gasification catalyst, it is characterized in that described catalyst comprises component A, B component, component C and coal sill, metal species in component A mass fraction in the catalyst is 1%-5%, metal species in B component mass fraction in the catalyst is 1%-5%, metal species in component C mass fraction in the catalyst is 1%-15%, remaining composition is mainly coal sill, and particle diameter is 40 mesh-80 mesh.
2. catalyst as claimed in claim 1, it is characterised in that described component A is one or more in nickel salt and iron salt.
3. catalyst as claimed in claim 1, it is characterised in that described B component is one or more in the calcium salt of solubility, magnesium salt, manganese salt and zinc salt.
4. catalyst as claimed in claim 1, it is characterised in that described component C is one or more in Organic Sodium Salt and potassium salt.
5. the catalyst as described in claim 1 or 4, it is characterised in that described component C is the one of which or several such as sodium lauryl sulphate, enuatrol, potassium oleate and polyacrylamide potassium salt.
6. as claimed in claim 1 for the preparation method of coal hydrogenation catalytic gasification catalyst, it is characterised in that: the mixing of component A, B component, component C and coal sill is placed in water by a., stirs；B. the mixture that step a prepares is added in autoclave, carry out hydrothermal treatment consists；C. the material in autoclave is taken out, carry out washing, dried；The most dried material is pressed into tablet.
7. the preparation method of catalyst as claimed in claim 6, it is characterised in that electrical conductivity of water used is less than 5 μ s/cm.
8. the preparation method of catalyst as claimed in claim 6, it is characterised in that hydrothermal treatment consists temperature is 80 DEG C ~ 200 DEG C, and pressure is 2.0MPa ~ 10.0MPa, and the time is 3h-5h.
9. catalyst as claimed in claim 1, is characterized in that being applied in the reaction of coal hydrogenation catalytic gasification preparing natural gas.
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Cited By (3)
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| CN109225234A (en) * | 2018-09-19 | 2019-01-18 | 石河子大学 | A kind of composition for carbon catalytic hydrogenation methane |
| WO2020088398A1 (en) * | 2018-10-29 | 2020-05-07 | 中国石油化工股份有限公司 | Pulverized coal preprocessing method and pulverized coal gasiifying method |
| CN114700080A (en) * | 2022-05-06 | 2022-07-05 | 武汉科技大学 | Coal gasification catalyst, loading method thereof and application of coal gasification catalyst in microwave gasification of low-rank coal |
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| CN109225234A (en) * | 2018-09-19 | 2019-01-18 | 石河子大学 | A kind of composition for carbon catalytic hydrogenation methane |
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Application publication date: 20170111 |